Category: 20850-43-5

Reference of 20850-43-5, 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. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, This compound has unique chemical properties. The synthetic route is as follows.

Taking 10 g about 89.7% content piperazine pyrimidine, 12 g triethylamine, 34 ml isopropanol into 100 ml three port into reaction, stirring at the room temperature under the chlorosilane dropping pepper, in 30 minutes in the transfusion. Heating to 50 C, thermal insulation 4 hours, stirring under cooling to room temperature, filter, recovery mother liquor, in the filter cake by adding 20 ml water beating, filtering, adding 10 ml water washes filters cake. 50 C drying, the crude product shall piribedil 16.6 g, HPLC analysis content 99.2%. Yield 92%

The chemical industry reduces the impact on the environment during synthesis 5-(Chloromethyl)benzo[d][1,3]dioxole. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Taicang Hongshan Environmental Protection Technology Co., Ltd.; Liu Lu; (9 pag.)CN107216318; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 20850-43-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 20850-43-5 name is 5-(Chloromethyl)benzo[d][1,3]dioxole, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

ake 10g about 89.7% content of piperazine pyrimidine, 12g triethylamine, 34ml isopropanol into 100ml three reaction flask, dropping peppermint chloride at room temperature under stirring, dropping over 30 minutes. Heated to 50 , incubated for 2 hours, cooled to room temperature with stirring, filtered, the mother liquor was recovered, the filter cake was added 20ml water beating, suction filtration, plus 10ml water washing cake. 50 drying, get piribedil crude 16.6g, HPLC analysis content of 99.2%. Yield 92%; 16g of crude piribedil (99.2%), 0.3g of activated charcoal and 42ml of absolute ethanol were added into a 100ml single-necked flask and heated to the reflux temperature for 0.5 hour. The activated carbon was removed by hot filtration and the filtrate was cooled and crystallized under stirring to obtain a white Crystalline solid. Filtered, rinsed with a small amount of anhydrous ethanol, and dried to obtain 14.76g of the first crystal product of piribedil, the content of which was 99.90% by HPLC and the refined yield was 90.33%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-(Chloromethyl)benzo[d][1,3]dioxole, and friends who are interested can also refer to it.

Reference:
Patent; Taicang Datang Chemical Fiber Factory; Liu Huifeng; (9 pag.)CN107266429; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 20850-43-5 as follows. Recommanded Product: 20850-43-5

General procedure: Suspension of the appropriate 3-amino-1,1-dioxo-1,4,2-benzodithiazine derivative 4a-h (0.5 mmol), anhydrous K2CO3 (1.5 mmol, 0.21 g) and the appropriate alkyl chloride (0.6 mmol) in dry THF (5 ml) was heated at reflux for 20-24 h, then cooled in ice-bath and filtered off. The crude product was suspended in 5 ml of water, heated gently to ca. 50 C; and cooled with vigorous stirring until granular precipitate appeared. Filtering off and washing with cold water and diluted EtOH gave pure potassium salts. 4.5.11 ;N-{2-[(1,3-Benzodioxol-5-yl)methylthio]-4-chloro-5-(3-phenyl-1,2,4-oxadiazol-5-yl)benzenesulfonyl}cyanamide potassium salt (5o) ;Starting from 4g (0.196 g) and 1,3-benzodioxol-5-ylmethyl chloride (0.102 g). Yield: 0.215 g (88%): m.p. 274-276 C; IR (KBr): nu 2923, 2179, 1625, 1585, 1560, 1500, 1488, 1362, 1349, 1253, 1226, 1143 cm-1; 1H NMR (500 MHz, DMSO-d6): delta 4.38 (s, 2H, SCH2), 6,01 (s, 2H, OCH2O), 6.90 (d, J = 7.81 Hz, 1H, Ar), 6.98 (d, J = 7.81 Hz, 1H, Ar), 7.05 (s, 1H, Ar), 7.59-7.63 (m, 3H, Ar), 7.70 (s, 1H, Ar), 8.10-8.11 (m, 2H, Ar), 8.59 (s, 1H, Ar); Anal. C23H14ClKN4O5S2 (C, H, N).

According to the analysis of related databases, 20850-43-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Brozewicz, Kamil; Slawinski, Jaroslaw; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 384 – 394;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 20850-43-5,Some common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, molecular formula is C8H7ClO2, 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.

To a slurry of magnesium turnings (1.09 g, 44.8 mmol) in 5 mL of THF was added iodine (0.0650 g, 0.256 mmol), followed by a solution of 5-(chloromethyl)benzo[d][l,3]dioxole (6.55 g, 38.4 mmol) in 30 mL of THF. After 1 minute, the exothermic reaction mixture was placed in an ice bath for 1 minute and then stirred at ambient temperature for 1 hour. TMEDA (7.68 ml, 51.2 mmol) was added to the reaction and the mixture was cooled to -78 0C for 5 minutes at which point a solution of (E)-N-((S)-2,3-bis(tert- butyldimethylsilyloxy)propylidene)-2-methylpropane-2-sulfinamide (5400 mg, 12.8 mmol) in 25 mL THF was added via a syring pump over 15 minutes. The reaction was allowed to warm to RT over the course of 2 hours then stirerd at RT for an additional hour. The mixture was diluted with ethyl acetate (100 mL) and poured in saturated ammonium chloride (250 mL). The aqueous layer was extracted with ethyl acetate (2 x 250 mL) and the combined organic layers were washed with water and then brine and dried over Na2SO4. The organic colvents were filtered, concentrated under reduced pressure and the crude material was purified by silica gel to provide N-((2R,3S)-1- (benzo[d][l,3]dioxol-5-yl)-3,4-bis(tert-butyldimethylsilyloxy)butan-2-yl)-2- methylpropane-2-sulfinamide (4.51 g, 63.1% yield) as a 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 5-(Chloromethyl)benzo[d][1,3]dioxole, its application will become more common.

Reference:
Patent; AMGEN INC.; WO2009/64418; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 20850-43-5, Quality Control of 5-(Chloromethyl)benzo[d][1,3]dioxole

Preparation of 13-benzodioxol-5-ylmetllel propyl sulfone 5. 0 g of 5-(chloromethyl)-1, 3-benzodioxol was dissolved in 20 ml of anhydrous tetrahydrofuran and 20 ml of diethyl ether and then added to magnesium at 0C, and reacted for 10 minutes. The reactant was heated to 50C and reacted for 1 hour. The reaction mixture was cooled to 0C and then slowly added to a flask containing [1, 3-bis (diphenylphosphino) propane] nickel (II) dichloride as a catalyst. After the addition of 2.8 ml propane sulfonyl chloride, the mixture was reacted for 30 minutes, then the reactant was heated to 50C and reacted for 1 hour. Then, its pH was adjusted to 7 with dilute hydrochloric acid. The resulting mixture was extracted with diethyl ether and distilled water, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was fractionated by column chromatography using ethyl acetate: n-hexane (1: 3), to give 0.8 g of the title compound of the following formula lc (Rf: 0.35, Yield: 7%). [Chemical Formula lc] The compound was dissolved in CDC13 and TMS and then characterized by H NMR spectroscopy. The result is as follows ; ‘H NMR S : 1. 16-1. 19 (t, 3H, J=7. 0Hz), 2.10-2. 15 (q, 2H, 7.4Hz), 2. 81 (s, 2H), 3.66-3. 69 (t, 2H, J=7.8Hz), 5.94 (s, 2H), 6.61-6. 63 (d of d, 1H), 6.68 (s, 1H), 7.28 (d, 1H, J=0.8).

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, 5-(Chloromethyl)benzo[d][1,3]dioxole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; HAN, Sang Min; LEE, Myung Hee; CHOI, Won Chul; WO2005/70915; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 20850-43-5, These common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, 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.

General procedure: A mixture of the required pyrrole-2-carboxylic acid ethylester 9-12 (3 mmol), sodium hydride (4.5 mmol) and theappropriate arylmethylchloride (4.5 mmol) in dry dimethylformamide(5 mL) was stirred at room temperature for 48hours; after this time water was added and the resultingcrude material was extracted with diethyl ether (3 50 mL).The combined organic layers were dried over anhydroussodium sulphate, filtered, and concentrated under reducedpressure; the obtained residue was purified by means of flashchromatography using a mixture of ethyl acetate/cyclohexane (2:8, v:v) as eluent. Oil compounds 19 and 20 (yield: 55 and 53%, respectively) were immediately usedwithout further purification for the next step. Using this procedure,the following compounds were obtained:

Statistics shows that 5-(Chloromethyl)benzo[d][1,3]dioxole is playing an increasingly important role. we look forward to future research findings about 20850-43-5.

Reference:
Article; Salerno, Loredana; Modica, Maria N.; Romeo, Giuseppe; Pittala, Valeria; Cagnotto, Alfredo; Siracusa, Maria A.; Medicinal Chemistry; vol. 11; 2; (2015); p. 109 – 117;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 20850-43-5, These common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, 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.

[[002511] To a mixture of 6-chloro-4- (3, 3-dimethyl-piperidin- 4-ylamino) -chromen-2-one, di-HBr salt (88 mg, 0.188 mmol) in THF was added Cs2CO3 (287 mg, 0.881 mmol) and the suspension was stirred for 5 min under nitrogen before 5-chloromethyl- benzo [[1,] 3] dioxole (124 mg, 0.363 mmol) was added dropwise. The mixture was stirred for 70 h at [25 C] before being refluxed 24 h. The reaction was concentrated with nitrogen flow. The crude product was partitioned between saturated aqueous [NAHC03] and EtOAc and the aqueous layer was extracted with EtOAc [(3X).] The combined organic layers were washed with saturated aqueous [NACL,] dried over [MGS04,] filtered, concentrated, and purified by C-18 RP LC-MS chromatography to afford 33 mg [(40%)] of the title compound as a white solid. MS (ESI (+) [Q1MS)] m/z 442 [(M+H)] + ; 1H NMR (300 MHz, DMSO) [B] ppm 0. [80] (s, 3H), 1. [06] (s, 3H), 1.52-1. 62 (m, [1H),] 1.84-2. 14 (m, 3H), 2.37-2. 55 (m, 1H), 2.80-2. 90 (m, 1H), 3.25-3. 37 (m, 1H), 3.39-3. 52 (m, 2H), 5.44 (s, 1H), 5.97-6. 02 (m, 2H), 6.73-6. 90 (m, 4H), 7.31-7. 38 (m, 1H), 7.60-7. 67 (m, 1H), 8.45-8. 50 (m, 1H).

Statistics shows that 5-(Chloromethyl)benzo[d][1,3]dioxole is playing an increasingly important role. we look forward to future research findings about 20850-43-5.

Reference:
Patent; MILLENNIUM PHARMACEUTICALS, INC.; WO2003/106452; (2003); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, A new synthetic method of this compound is introduced below., HPLC of Formula: C8H7ClO2

2-(Methylamino)ethanol (22.0 g, 290 mmol) is added all at once to a stirred solution of 3,4-methylenedioxybenzyl chloride (25.0 g, 147 mmol) in DCM (45 mL) at -78 C. under nitrogen. The solution is stirred for 15 minutes at -78 C. then allowed to warm to room temperature overnight (16 h). The reaction is quenched with 1.2 M NaOH (100 mL), washed twice with water, dried of MgSO4, and filtered. Concentration under reduced pressure afforded 25.3 g (83%) of 2-(benzo[1,3]dioxol-5-ylmethyl-methyl-amino)-ethanol as a clear oil which was suitable for use in the next step.

The synthetic route of 20850-43-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kalypsys, Inc.; US2006/116515; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 20850-43-5, 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. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

5- (chloromethyl) prepared in Step 1 of Example 31 under an argon atmosphere benzo [d] [1,3] dioxole (2.29 g, 13.42 mmol)Was dissolved in acetonitrile (27 mL) The N- bromo succinimide polyimide (2.39 g, 16.11 mmol) was dissolved inRespectively. The reaction solution was stirred at room temperature for 13 hours,The completion of the reaction was monitored by TLC (hexane:Ethyl acetate = 2: 1).The reaction mixture was poured into water,The organic solvent layer extracted with dichloromethane (10 mL x 3) was washed again with a saturated solution of sodium chloride (50 mL), and the organic solvent layer was dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to remove the solvent. The concentrate was separated and purified by column chromatography (hexane: ethyl acetate = 5: 1) to obtain the desired compound (3.32 g, 99% yield).

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, 5-(Chloromethyl)benzo[d][1,3]dioxole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Korea Institute of Science and Technology; Kim Eun-gyeong; Keum Gyo-chang; Lee Ju-hyeon; Shin Sang-cheol; Seo Seon-hui; (39 pag.)KR2018/40037; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 20850-43-5, These common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, 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.

General procedure: Suspension of the appropriate 3-amino-1,1-dioxo-1,4,2-benzodithiazine derivative 4a-h (0.5 mmol), anhydrous K2CO3 (1.5 mmol, 0.21 g) and the appropriate alkyl chloride (0.6 mmol) in dry THF (5 ml) was heated at reflux for 20-24 h, then cooled in ice-bath and filtered off. The crude product was suspended in 5 ml of water, heated gently to ca. 50 C; and cooled with vigorous stirring until granular precipitate appeared. Filtering off and washing with cold water and diluted EtOH gave pure potassium salts. 4.5.6 ;N-{2-[(1,3-Benzodioxol-5-yl)methylthio]-4-chloro-5-[5-(4-chlorophenyl)-1,3,4-oxadiazol-2-yl]benzenesulfonyl}cyanamide potassium salt (5j) ;Starting from 4b (0.214 g) and 1,3-benzodioxol-5-ylmethyl chloride (0.102 g). Yield: 0.240 g (80%): m.p. 308-310 C; IR (KBr): nu 3436, 3086, 2924, 2172, 1602, 1585, 1543, 1502, 1486, 1327, 1289, 1253, 1141 cm-1; 1H NMR (500 MHz, DMSO-d6): delta 4.36 (s, 2H, SCH2), 6.01 (s, 2H, OCH2O), 6.88-7.04 (m, 5H, Ar), 7.68 (s, 1H, Ar), 7.70 (m, 2H, Ar), 8.08-8.09 (m, 2H, Ar), 8.47 (s, 1H, Ar); Anal. C23H13Cl2KN4O5S2 (C, H, N).

Statistics shows that 5-(Chloromethyl)benzo[d][1,3]dioxole is playing an increasingly important role. we look forward to future research findings about 20850-43-5.

Reference:
Article; Brozewicz, Kamil; Slawinski, Jaroslaw; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 384 – 394;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics