Sep-21 News Continuously updated synthesis method about 10061-02-6

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Synthetic Route of 10061-02-6, A common heterocyclic compound, 10061-02-6, name is trans-1,3-Dichloropropene, molecular formula is C3H4Cl2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Eine geruehrte Loesung von 77,7 ml Diisopropylamin und 200 ml Tetrahydrofuran wird auf -20 C gekuehlt und waehrend 15 Minuten mit 200 ml 2,5 M n-Hexyllithiumloesung (in Hexan) versetzt. Die Loesung wird 15 Minuten bei -20 C nachgeruehrt und anschliessend wird waehrend 30 Minuten eine Loesung von 75,3 ml Isovaleriansaeureethylester in 80 ml Tetrahydrofuran zugetropft. Die Loesung wird 10 Minuten nachgeruehrt und dann waehrend 10 Minuten bei -20 C mit 80 ml DMPU versetzt. Zugabe von 8,2 g Natriumiodid und 19,5 g trans-1,3-Dichlorpropen. Das Reaktionsgemisch wird noch 23 Stunden bei – 20 C nachgeruehrt und anschliessend mit 500 ml 20%-iger waessriger Ammoniumchloridloesung versetzt. Die Mischung wird mit tert.-Butylmethylether (2x 400 ml) extrahiert und die organischen Phasen nacheinander mit 0,1 M Natriumthiosulfatloesung (1x 500 ml), Wasser (1x 500 ml) und Sole (1x 500 ml) gewaschen. Die vereinigten organischen Phasen werden mit 150 g Natriumsulfat getrocknet und eingedampft. Aus dem Rueckstand wird mittels Destillation die Titelverbindung A1 als farbloses Oel erhalten (86,1 g, 84 %). 1H-NMR (400 MHz, CDCl3, delta) : 0,95 (m, 6H), 1,30 (t, 3H), 1,92 (m, 1H), 2,20 – 2,40 (m, 3H), 4,20 (m, 2H), 5, 80 – 6,10 (m, 2H) ppm.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Speedel Pharma AG; EP1200384; (2004); B1;,
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Application of 10061-02-6

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, trans-1,3-Dichloropropene, other downstream synthetic routes, hurry up and to see.

Reference of 10061-02-6, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 10061-02-6, name is trans-1,3-Dichloropropene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 1.22 g (0.011 mol) of (E)-1,3-dichloropropene 6, 2.07 g(0.015 mol) of K2CO3, 50 mL of anhydrous acetonitrile, and 2.88 g (0.01 mol) of 1-[bis(4-fluorophenyl)-methyl]piperazine 5 was stirred for 0.5 h at room temperature, and then for 4 h under reflux until amine 5 was completely consumed (monitoring with GLC). After cooling, the solution was filtered, and the precipitate was washed with ethyl acetate. The combined organic layers were concentrated, and the residue was purified by column chromatography (hexane-ethylacetate, 9 : 1 ? 2 : 1). Yield 3.31 g (91%), colorless crystals, mp 89C. IR spectrum, nu, cm-1: 1609, 1506,1453, 1288, 1226, 1153, 1137, 1008, 828. 1 NMRspectrum, delta, ppm: 2.43 br.s (4H, CH2N), 2.51 br.s (4H,CH2N), 3.04 d (2H, CH2CH=, J = 7.0 Hz), 4.23 s (1H,HAr2), 5.98 d.t (1H, CH2CH=, Jtrans = 13.2, 7.0 Hz),6.15 d (1H, ClCH=, Jtrans = 13.2 Hz), 6.96 t (4H, CHAr,J = 8.5 Hz), 7.28-7.38 m (4H, CHAr). 13 NMR spectrum,delta, ppm: 51.51 (2CH2N), 52.97 (2CH2N), 58.10(C1), 74.33 (HAr2), 115.13 d (4CHAr, 2JCF = 20 Hz),120.59 (C3), 129.20 d (4CHAr, 3JCF = 6.8 Hz), 129.96(C2), 138.11 (2CAr), 161.78 d (2CFAr, 1JCF = 244.2 Hz).Mass spectrum, m/z (Irel, %): 362 (0.8) [M]+, 203 (41),201 (19), 183 (30), 161 (31), 159 (100), 132 (13), 123(32), 75 (34), 56 (15), 42 (22). Mass spectrum(HRMS), m/z: 362.1348 [M]+ (calculated forC20H21ClF2N2: 362.1361).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, trans-1,3-Dichloropropene, other downstream synthetic routes, hurry up and to see.

Reference:
Letter; Shakhmaev; Sunagatullina, A. Sh.; Zorin; Russian Journal of General Chemistry; vol. 86; 8; (2016); p. 1969 – 1972; Zh. Obshch. Khim.; vol. 86; 8; (2016); p. 1395 – 1398,4;,
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The important role of trans-1,3-Dichloropropene

According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 10061-02-6, name is trans-1,3-Dichloropropene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C3H4Cl2

To a 500 ml round bottom flask was charged 7-fluoro-6-nitrobenzoxazin-3-one (12.73 g, 0.060 mol) and potassium carbonate (9.95 g, 0.072 mol)Dissolved in 60 ml of N,N-dimethylformamide to form a suspension,Heating to 80 C,After the reaction was kept at this temperature for 30 minutes,(E)-1,3-dichloropropene (8.00 g, 0.072 mol) was added dropwise thereto.The reaction was maintained at 80 C for an additional 4 hours. After stopping the reaction,Cool naturally to room temperature and pour into 200 ml of water.After extraction with ethyl acetate (100 ml × 3), the combined organic phases were washed with saturated aqueous sodium chloride (50 ml × 3), dried over anhydrous magnesium sulfate Ester: petroleum ether = 1:3) 12.20 g of (E)-4-(3-chloroallyl)-7-fluoro-6-nitrobenzoxazin-3-one as a yellow solid, yield 71 %.

According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shenyang Sinochem Pesticide Chemical Research And Development Co., Ltd.; Li Bin; Chen Lin; Cui Dongliang; Guo Zhengfeng; Ma Hongjuan; Lian Weixiang; (23 pag.)CN109836393; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

The important role of 10061-02-6

According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.

Synthetic Route of 10061-02-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 10061-02-6 as follows.

EXAMPLE 1; 382 g (406 ml) of DMF were initially charged in a Schmizzo and 137 g (141 ml) of 1.0 eq. NaOMe (30% solution in methanol) were added. This mixture was then heated to 60 C. (+/-3 C.) and 131 g (0.753 mol) of dimethyl isopropylmalonate were metered in within one hour. Subsequently, a methanol/DMF mixture (201 g) was distilled off under pressure (300 mbar to 60 mbar) and a temperature of 60 C.Thereafter, at 80 C. (+/-3 C.), 86 g (79 ml, 0.779 mol, 1.03 eq.) of 1,3-dichloropropene were metered in within one hour and the reaction mixture was then heated at 80 C. (+/-3 C.) for two hours. The reaction mixture was heated to 140 C. and a 25% solution of LiCl (0.6 eq.) in methanol (19 g of LiCl in 58 g of methanol) was metered in within two hours, and the reaction mixture was heated at 140-142 C. for a further 6 hours, in the course of which a portion of the methanol was distilled off and approx. 1.5 mol of gas (mainly CH3Cl and CO2) formed. The maximum amount of gas in the first half hour was approx. 6 liters. On completion of reaction, the solvent (DMF) and the excess methanol were distilled off substantially fully under reduced pressure. The remainder was admixed with 200 g of water, 89 g of 34% HCl and 200 g of MTBE, and the phases were separated. The organic phase was washed lx with 50 g of water and the solvent was removed under reduced pressure. Approx. 140 g of product were obtained, of which approx. 125 g were ester and 13 g the corresponding acid.

According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DSM Fine Chemicals Austria NFG GMBH & Co KG; US2008/207943; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

New downstream synthetic route of 10061-02-6

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 10061-02-6, its application will become more common.

Some common heterocyclic compound, 10061-02-6, name is trans-1,3-Dichloropropene, molecular formula is C3H4Cl2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Safety of trans-1,3-Dichloropropene

Example 3 (E)-2-(1-Methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methyl-6-(3-chloroprop-2-enyloxy)pyridine A mixture of 6-hydroxy-2-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methylpyridine (0.9 g, 3.3 mmol) and NaH (60 % in oil, 0.16 g, 4 mmol) in acetonitrile (20 ml) and DMF (1 ml) is stirred for 10 min at ambient temperature and (E)-1,3-dichloropropene (0.4 g, 3.6 mmol) is added. After stirring for 60 h at ambient temperature, the remaining NaH is deactivated and the resulting mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed with water. The organic layer is dried with anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v) yields the title compound (0.6 g, 52 % yield) as an colorless oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 10061-02-6, its application will become more common.

Reference:
Patent; American Cyanamid Company; EP955300; (1999); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

New downstream synthetic route of 10061-02-6

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 10061-02-6, its application will become more common.

Some common heterocyclic compound, 10061-02-6, name is trans-1,3-Dichloropropene, molecular formula is C3H4Cl2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Safety of trans-1,3-Dichloropropene

Example 3 (E)-2-(1-Methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methyl-6-(3-chloroprop-2-enyloxy)pyridine A mixture of 6-hydroxy-2-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methylpyridine (0.9 g, 3.3 mmol) and NaH (60 % in oil, 0.16 g, 4 mmol) in acetonitrile (20 ml) and DMF (1 ml) is stirred for 10 min at ambient temperature and (E)-1,3-dichloropropene (0.4 g, 3.6 mmol) is added. After stirring for 60 h at ambient temperature, the remaining NaH is deactivated and the resulting mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed with water. The organic layer is dried with anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v) yields the title compound (0.6 g, 52 % yield) as an colorless oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 10061-02-6, its application will become more common.

Reference:
Patent; American Cyanamid Company; EP955300; (1999); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Discovery of trans-1,3-Dichloropropene

According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.

Electric Literature of 10061-02-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 10061-02-6 as follows.

11h were made from corresponding terminal alkyne and vinyl chloride S139 via route shown in Scheme 7. To a solution of S13 (600mg, 3.04 mmol ) in CH3CN was added K2CO3 (4.2g, 30.4 mmol) and continue stirred half of a hour, then added S9 (1g, 9.13 mmol) at room temperature, after the solution was heated at 40 C for 7h. The reaction was filter, and concentrated in vacuo. Purification via flash chromatography on silica gel(PE/EA = 20/1) provided S14( 490 mg,60% yield).Pd(PPh3)4 (97 mg, 0.084 mmol) andcopper iodide (32 mg, 0.169 mmol) were added to a seal-tube.Absorb the air andfill with nitrogen.S14 (460 mg, 1.69mmol) , prop-2-yn-1-ylbenzene ( 224 mg, 2.03 mmol ), tert-butylamine (185 mg,2.54 mmol) and 8 mL toluene was added.The mixture was heated to 70 C and stirred for 6 h. The reaction was thencooled and diluted with Et2O (10 mL) and saturated aqueous NH4Cl(5 mL). The organics were extracted with Et2O (2 *10 mL), dried overNa2SO4, filtered, and concentrated in vacuo. Purification via flash chromatography on silica gel (PE/EA = 10/1) provided 11h (317mg, 65% yield).

According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Xu, Hua-Dong; Wu, Hao; Jiang, Chun; Chen, Peng; Shen, Mei-Hua; Tetrahedron Letters; vol. 57; 26; (2016); p. 2915 – 2918;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

The important role of trans-1,3-Dichloropropene

According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 10061-02-6 as follows. SDS of cas: 10061-02-6

Example 15: N-((S)-2-Amino-l-hydroxycarbamoyl-2-methyl-propyl)-4-((E)-7-hydroxy- hept-2-en-4-ynyIoxy)-benzamide (Compound 15); 15Step 15-A:To a solution of trans- 1,3 -dichloropropene (2.19 g, 19.7 mmol), potassium carbonate (3.63 g, 26.3 mmol), and potassium iodide (0.109 g, 0.657 mmol) in acetonitrile (200 mL) was added methyl-4-hydroxybenzoate (2.0 g, 13.2 mmol). The reaction was stirred at 80 0C for 4 hr after which it is quenched with brine, extracted with ethyl acetate, and washed with water. Organic phase dried with anhydrous magnesium sulfate, filtered, concentrated followed by purification with silica-gel chromatography (0-50% Ethyl Acetate/Heptane) to afford 15b (2.77 g). Found m/z ES+ = 227.

According to the analysis of related databases, 10061-02-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NOVARTIS AG; DOBLER, Markus, Rolf; LENOIR, Francois; PARKER, David, Thomas; PENG, Yunshan; PIIZZI, Grazia; WATTANASIN, Sompong; WO2010/31750; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Share a compound : trans-1,3-Dichloropropene

The synthetic route of 10061-02-6 has been constantly updated, and we look forward to future research findings.

10061-02-6, name is trans-1,3-Dichloropropene, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Computed Properties of C3H4Cl2

(1), the (E)- 1, 3 – dichloropropene (354g, 3.20 muM) added to the tetrahydrofuran (1.5L) solution, light added under mixing sodium iodide (595g, 3.2 muM), stirring at the room temperature 2h, preparation of (E)-1 – chloro -3 – iodo propylene reaction liquid for use. The (S)-4 – phenyl -2 oxazolidone (720g, 2.91 mol) is added to the tetrahydrofuran (2L) solution, lowering the temperature to -10 C, dropwise 1N II (trimethyl silicon-based) amino lithium (486.8g, 2 . 91 muM) tetrahydrofuran solution (3L), to maintain the temperature of the reaction solution is lower than the -10 C, after the completion of the dropping -10 C reaction 2h, then adding the above-mentioned preparation of (E)-1 – chloro -3 – iodo acrylic solution. Then slow heating to 10 C, overnight reaction. TLC monitoring raw material the reaction is complete. The reaction liquid is poured into the saturated NH4Cl solution (5L) quenching, steaming and remove a portion of the solvent, and then the extraction of ethyl acetate concentrate (2L × 3), combined with the several phase, anhydrous sodium sulfate drying, steaming and to job 1 kg brown oily matter, directly used for the next step reaction.

The synthetic route of 10061-02-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Borui Bio-pharmaceutical (Suzhou) Co., Ltd.; Yuan Jiandong; Liu Wei; Ma Shimin; (29 pag.)CN104058990; (2017); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Continuously updated synthesis method about 10061-02-6

Statistics shows that trans-1,3-Dichloropropene is playing an increasingly important role. we look forward to future research findings about 10061-02-6.

Related Products of 10061-02-6, These common heterocyclic compound, 10061-02-6, name is trans-1,3-Dichloropropene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Potassium hydroxide (32.2 g) and toluene (250 mL) were taken into a round bottom flask and stirred for about 10 minutes. Dimethylisopropyl malonate (50 g) and tetrabutylammonium bromide (10 g) were then added to it and again stirred for about 10 minutes, trans-lambda ,3-Dichloropropene (35 g) was added to the reaction mixture and maintained at about 30-35 C for about 4 hours. After the reaction was completed, the reaction mass was quenched with water (500 ml_) and stirred for about 10 minutes. The reaction mixture was extracted into toluene (250 ml_), and the toluene layer was washed with water and then evaporated under reduced pressure to afford 51 g (82% yield) of (£)-dimethyl 2- (3-chloroallyl)-2-isopropylmalonate as a dark brown viscous liquid. Purity by GC: 96.84%

Statistics shows that trans-1,3-Dichloropropene is playing an increasingly important role. we look forward to future research findings about 10061-02-6.

Reference:
Patent; DR. REDDY’S LABORATORIES LTD.; DR. REDDY’S LABORATORIES, INC.; KOLLA, Naveen Kumar; APPAYE, Kaliyaperumal Srinivasan; GANGULA, Srinivas; GOVINDAPUR, Rajeshwar Reddy; MANNE, Nagaraju; NIKUMBH, Satish Pandurang; NEELAM, Uday Kumar; JOSEPH, Suju Chuttippari; BADDAM, Sudhakar Reddy; KUNHIMON, Shyam Kumar Unniaranpurakkal; MOOVENDAN, Mohan; DAHANUKAR, Vilas; DONIPARTHI, Kiran Kumar; WO2012/21446; (2012); A2;,
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