Tag: M.W=100-200

348-59-4, 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 348-59-4 as follows.

Step 1 a) The mixture of 1 ,4-dichloro-2-fluoro-benzene (5.4 g, 0.0327 mol), AICI3 (10.4 g, 0.0784 mol) was warmed to 60 C, and acetyl chloride (3.85 g, 0.0491 mol) was added by syringe over 5 min under N2, the mixture was warmed to 100 C for 2h. Then the mixture was added into ice water and adjusted pH to 2 by 1 N HCI. Extracted by MTBE (100 ml*2), dried and concentrated to give 1 – (2,5-dichloro-4-fluoro-phenyl)ethanone (6g, crude). 1H NMR : CDCI3 400MHz, delta (ppm)= 2.58 (s, 3 H), 7.19 (d, J=8.38 Hz, 1 H), 7.63 (d, J=7.94 Hz, 1 H).

According to the analysis of related databases, 2,5-Dichlorofluorobenzene, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BASF SE; GRAMMENOS, Wassilios; CRAIG, Ian Robert; BOUDET, Nadege; MUeLLER, Bernd; DIETZ, Jochen; LAUTERWASSER, Erica May Wilson; LOHMANN, Jan Klaas; GROTE, Thomas; HADEN, Egon; ESCRIBANO CUESTA, Ana; WO2014/82879; (2014); A1;,
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26487-67-2, 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. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 1,1-bis(4-hydroxyphenyl)-2-cyclohexyl-2-phenylethene (37.6 mg, 0.101 mmol) in DMF (1.02 mL) at 0 ¡ãC was added 60percent sodium hydride (dispersion in paraffin liquid, 24.4 mg, 0.610 mmol). The reaction mixture was stirred for 15 min at 50 ¡ãC and then N-(2-chloroethyl)hexahydro-1H-azepine hydrochloride (66.4 mg, 0.335 mmol) was added in portions at room temperature. After the reaction mixture had been stirred for 15.5 h at 50 ¡ãC, saturated aqueous ammonium chloride was added at 0 ¡ãC. The mixture was extracted with dichloromethane and the organic layer was dried over sodium sulfate. After filtration of the mixture and evaporation of the solvent, the crude product was purified by thin layer chromatography on silica (eluant; ammoniacal chloroform/methanol = 9/1) to afford RID-F-S*13 (compound 9) (51.9 mg, 83percent) as a pale yellow oil

The synthetic route of 26487-67-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hasegawa, Makoto; Yasuda, Yukari; Tanaka, Makoto; Nakata, Kenya; Umeda, Eri; Wang, Yanwen; Watanabe, Chihiro; Uetake, Shoko; Kunoh, Tatsuki; Shionyu, Masafumi; Sasaki, Ryuzo; Shiina, Isamu; Mizukami, Tamio; European Journal of Medicinal Chemistry; vol. 71; (2014); p. 290 – 305;,
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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 1871-57-4 as follows. 1871-57-4

To sodium hydride (60 wt.% in mineral oil, 2.464 g, 61.6 mmol) in DMF (50 mL) was added 3-chloro-2-(chloromethyl)prop-l-ene (3.5 g, 28.0 mmol) at ~5 C (ice bath) and a solution of tert-butyl(2-hydroxyethyl)carbamate (4.51 g, 28.0 mmol) in tetrahydrofuran (50 mL). The reaction mixture was stirred at 20-30 C for ~2 hrs and concentrated under reduced pressure to remove tetrahydrofuran. The resulting mixture was poured into water and extracted with EtOAc. The combined organic extracts were washed with brine, dried over sodium sulfate, filtered off and concentrated under reduced pressure. The residue was purified by column chromatography [silica gel, 80 g, EtO Ac/heptane = 0/100 to 50/50] providing tert-butyl 6-methylene-l ,4-oxazepane-4- carboxylate (4 g) as a colorless oil. NMR (400 MHz, chloroform-d) delta [ppm]: 1.46 (s, 9 H) 3.33 – 3.62 (m, 2 H) 3.62 – 3.82 (m, 2 H) 4.09 (m, 2 H) 4.16 (m, 2 H) 4.99 (m,2 H).

According to the analysis of related databases, 1871-57-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NOVARTIS AG; PFISTER, Keith B; SENDZIK, Martin; WO2011/26917; (2011); A1;,
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83121-15-7, Name is 3,5-Dichloro-2,4-difluoroaniline, 83121-15-7, 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.

Example 10 N-(2,4-Difluoro-3,5-dichlorophenyl)-N’-(2,6-difluorobenzoyl)-urea Three grams (0.016 mol) of 2,6-difluoro-benzoyl isocyanate were added to a solution of 2.95 gm (0.015 mol) of 2,4-difluoro-3,5-dichloroaniline in 50 ml of toluene. The solution thus obtained was stirred for 15 hours at room temperature. Thereafter, the product which precipitated during that time was removed by suction filtration and dried. Yield: 4.2 gm (0.011 mol; 73% of theory), M.p.: 221-224 C.

Statistics shows that 3,5-Dichloro-2,4-difluoroaniline is playing an increasingly important role. we look forward to future research findings about 83121-15-7.

Reference:
Patent; Celamerck GmbH & Co. KG; US4457943; (1984); A;,
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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 2533-69-9 as follows. 2533-69-9

24. 55 mmol of PHENYLENEDIAMINE 1a-k, 1M, In were dissolved in 50 ml of acetic acid, AND 27 MMOL of methy 2, 2, 2-TRICHFOROACETIMIDATE 2 WERE added at 0C over the course of 0.5 hour under an N2 atmosphere. When the addition was complete, the reaction mixture was slowly warmed to room temperature and stirred at this temperature for 2 hours. The reaction mixture was poured into ice-water, and the resulting precipitate was filtered off with suction, washed with a little water and dried at 40C under reduced pressure. 3a: R = 5-Cl ; brown solid, yield : 82%

According to the analysis of related databases, 2533-69-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK PATENT GmbH; WO2005/4863; (2005); A1;,
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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 6223-78-5 as follows. 6223-78-5

In a 250 ml_ round-bottomed flask was weighed T-1 (1.8 g, 10 mmol). Dry DCE (20 ml_) was added followed by dry toluene (921 mg, 10 mmol, 1 equiv). Then AICI3 (133 mg, 1 mmol, 10 mol%) was added in portions. The resulting mixture was stirred under argon for 16 h. The mixture was cooled to room temperature, and then poured on ice-water (50 ml_). The organic layer was separated and the aqueous layer was extracted with Et2Patent; QUEEN’S UNIVERSITY AT KINGSTON; CAMERON, Donald Andrew; PETKOVICH, Martin; RANTANEN, Toni Kristian; SNIECKUS, Victor; BOARD, Johnathan; SINGH, Suneel; MAHETA, Ashishkumar Jayantilal; (76 pag.)WO2018/107289; (2018); A1;,
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2729-34-2, 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. 2729-34-2, name is 3,5-Dichloro-4-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows.

A solution of 3,5-dichloro-4-fluoroaniline (1 g, 5.58 mmol) in con. HC1 (20 mL) was cooled to 0-5 C. A solution of sodium nitrite (424 mg, 6.14 mmol) in water (1 mL) was added dropwise over 20 min with stirring. The resulting solution was stirred for 1 h at 0-5 C. Potassium ethyl xantogenate (1.33 g, 8.37 mmol) was added and the reaction mixture was stirred at 70 C overnight. The resulting solution was extracted with EtOAc (20 mL x 3). The combined organic layers were washed with brine (20 mL), dried over Na2S04, and concentrated in vacuum to give crude product, which was purified by FC to afford crude product. The crude product dissolved in EtOH (20 mL) followed by addition of 2M NaOH(5.6 mL). The mixture was stirred at 70 C for 2h. The mixture was extracted with DCM(30 mL) and the water layer pH was adjusted to pH5-6 by NaHSCL aq. followed by addition of DCM (30 mL). The organic layer was isolated and was washed, dried over sodium sulphate and concentrated to dryness to give the title compound 90.2 mg which was used in the next step without further purification m/z calcd for [C6H3Cl2FS]+ [M-H] : 195.0; found: 195.0.

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Reference:
Patent; GALECTO BIOTECH AB; ZETTERBERG, Fredrik; (118 pag.)WO2019/137971; (2019); A1;,
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108-70-3, The chemical industry reduces the impact on the environment during synthesis 108-70-3, name is 1,3,5-Trichlorobenzene, I believe this compound will play a more active role in future production and life.

General procedure: An oven-dried and argon-flushed pressure tube was charged with 1,3,5-trichlorobenzene, 1,2,4-trichlorobenzene or 1,2,3-trichlorobenzene (0.25 mmol), Pd2(dba)2 (1.25 mol%), cataCXium A (5.0 mol%), boronic acid (1.5 mmol) and K3PO4 (1.5 mmol) followed by anhydrous toluene (4.0 mL). The tube was sealed with a Teflon valve and the reaction mixture was stirred at 110 C for 24 h. The cooled reaction mixture was diluted with water and extracted with DCM. The combined organic layers were dried (Na2SO4), filtered and the filtrate was concentrated in vacuo. The residue was purified by column chromatography.

The chemical industry reduces the impact on the environment during synthesis 1,3,5-Trichlorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Article; Reimann, Sebastian; Ehlers, Peter; Sharif, Muhammad; Spannenberg, Anke; Langer, Peter; Tetrahedron; vol. 72; 8; (2016); p. 1083 – 1094;,
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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.

Step (b): After the step (a), the reaction system was cooled to 90C, and (1E)-1,3-dichloro-1-propene (192.3 g) in toluene (250 ml) was added. After 2 hours of heating with stirring, the system was cooled to 50C, and water was added to terminate the reaction. The aqueous layer was extracted with diisopropyl ether (IPE), and the extract was combined with the organic layer and washed with water and 5% aqueous NaCl, successively. The solvent was evaporated under reduced pressure to give dimethyl 2-[(2E)-3-chloro-2-propenyl]-2-isopropylmalonate (409.7 g). The product contained 87% (GC purity) of dimethyl 2-[(2E)-3-chloro-2-propenyl]-2-isopropylmalonate and at most 0.5% (measured by GC) of isopropyl bromide, but did not contain the Z-isomer. 1HNMR (400 MHz, CDCl3): 0.98 (d, 6H, J=6.76), 2.31 (m, 1H), 2.62 (dd, 2H, J=1.16, 7.64), 3.73 (s, 6H), 5.89 (dt, 1H, J=7.60, 13.19), 6.01 (dt, 1H, J=1.16, 13.19). 13CNMR (400 MHz, CDCl3): 18.33, 32.41, 35.14, 51.94, 62.06, 119.83, 128.87, 170.66.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 10061-02-6.

Reference:
Patent; ASAHI GLASS COMPANY LTD.; EP1571138; (2005); A1;,
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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. 2106-02-7, name is 2-Chloro-4-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., 2106-02-7

Under nitrogen protection, a water separator was installed in a 2L four-necked flask, and 145.5 g of 2-chloro-4-fluoroaniline and 130 g of 4-methoxybenzaldehyde were added.Concentrated sulfuric acid 20.0g and 1.2L of toluene, Reflux water separation reaction 6h, no obvious water droplets in the water separator can stop the reaction.After cooling to room temperature, it was washed with 100 mL of 10% aqueous sodium hydroxide solution, and the organic phase was decomposed under reduced pressure.The residue obtained was distilled under reduced pressure of 10 mmHg to give the titled product, N-(4-methoxybenzylidene)-2-chloro-4-fluoroaniline, 243.9 g, gas chromatographic content 99.4%, yield 92.5%.

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Reference:
Patent; Shanghai Kangpeng Technology Co., Ltd.; Zeng Yuan; Zhou Yan; Li Bolan; Chen Xiaobin; Wang Daoxiang; Yang Jianhua; (19 pag.)CN108276294; (2018); A;,
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