Month: March 2021

Adding a certain compound to certain chemical reactions, such as: 72934-36-2, name is 1-(4-Chlorophenyl)cyclopropanamine, 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 72934-36-2, Recommanded Product: 72934-36-2

To a stirred solution of 1 -benzyl 3 -((3aR ,5aR ,5bR ,7aR ,95, 11 aR, 1 ibR, 1 3a5)-3a-iso cyanato- 1 -isopropyl-5a,5b,8,8, 11 a-pentamethyl-2-oxo-3 ,3a,4,5,5a,5b,6,7,7a,8,9, 10,11,11 a, 1 ib, 12,13,1 3a-octadecahydro-2H-cyclopenta[ajchrysen-9-yl) (1R,35)-2,2-dimethylcyclo butane-i,3-dicarboxylate (Intennediate-2, 3.0 g, 4.213 mmol, 1.0 eq) in THF (30 ml) wasadded DIPEA (2.16 ml, 12.64 mmol, 3.0 eq) followed by i-(4-chlorophenyl)cyclopropan-i- amine (Intennediate-4, 0.847 g, 5.056 mmol, 1.2 eq). The reaction mixture was stirred at room temperature for about 16 hours. TLC indicated starting material was consumed and the desired product was observed. The reaction mixture was diluted with water (75 ml) andextracted with ethyl acetate (3×75 ml). The combined organic extracts were washed with water (75 ml) and brine solution (50 ml). The organic layer was dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by silicagel column chromatography by using 0-2% methanol in dichloromethane gradient. The fractionscontaining the expected product were combined and concentrated under reduced pressure to give the desired product (3.0 g, 80.9% yield) as a white solid. ?H NMR (300 MHz, CDC13): ppm 7.37-7.34 (m, 5H), 7.30 (d, J = 8.7 Hz, 2H), 7.13 (d, J = 8.7 Hz, 2H), 5.16, 5.10 (ABq, JAB= 12.3 Hz, 2H), 5.09 (s, 1H), 4.76 (s, 1H), 4.44 (dd, J= 11.4, 4.8 Hz, 1H), 3.18-3.07 (m, 1H), 2.87-2.57 (m, 5H), 2.20 (d, J = 18.3 Hz, 1H), 2.14-1.98 (m, 2H), 1.91-1.80 (m, 2H),1.80-1.61 (m, 4H), 1.56-1.39 (m, 4H), 1.39-1.25 (m, 6H), 1.34 (s, 3H), 1.22 (s, 3H), 1.19 (s,3H), 1.17-1.0 (m, 4H), 0.97 (s, 3H), 0.91 (s, 3H), 0.88 (s, 3H), 0.85 (s, 6H), 0.79 (m, 1H),0.75 (s, 3H); ESI-MS: mlz 901.46 (M+Na)t

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; HETERO RESEARCH FOUNDATION; BANDI, Parthasaradhi Reddy; KURA, Rathnakar Reddy; GAZULA LEVI, David Krupadanam; ADULLA, Panduranga Reddy; KASIREDDY, Bhaskar Reddy; (84 pag.)WO2017/64628; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 6940-78-9, A common heterocyclic compound, 6940-78-9, name is 1-Bromo-4-chlorobutane, molecular formula is C4H8BrCl, 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.

[0096] A mixture of beta-naphthol (1gm, 0.006 mole), anhydrous K2CO3 (10 gm, in excess) and 1-bromo 4-chlorobutane (0.8 ml, 0.006 mole) was refluxed in dry acetone (50 ml) for 6 hours. Reaction mixture was filtered and filtrate was concentrated to get oily compound, which was crystallized with benzene-hexane to give the colorless crystals of pure desired compound, m.p. 112 C., (yield 1.6 gm, 98%).

The synthetic route of 6940-78-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH; US2004/192688; (2004); A1;,
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. 10272-06-7, name is 3-Chloro-5-methoxyaniline, A new synthetic method of this compound is introduced below., Safety of 3-Chloro-5-methoxyaniline

To a solution of compound obtained from Step c (0.1 g, 0.3003 mmoles) in 7V,7V- dimethylformamide (1 ml) were added 1 -hydroxy benzotriazole (0.04 g, 0.3003 mmoles), N-ethyldiisopropyl amine (0.116 g, 0.9009 mmoles) and 3-chloro-5-methoxyaniline (0.047 g, 0.3003 mmoles) at room temperature. The reaction mixture was allowed to stir at room temperature for about 5 minutes and then l-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.086 g, 0.4505 mmoles) was added to it. The reaction mixture was again stirred at room temperature for about 12 hours. After completion, the solvent was evaporated under vacuum, diluted with water and extracted with ethyl acetate. The resulting organic layer was washed with water, dried over anhydrous sodium sulphate, filtered and evaporated under vacuum to afford an oily residue which was purified through flash column chromatography eluting with ethyl acetate :dichloromethane (3:7) to afford the title compound as white solid. Yield: 0.07g.1H NMR (400 MHz, DMSO-i? delta: 9.48 (s, 1H), 7.82 – 7.88 (m, 2H), 7.37 – 7.44 (m, 2H), 7.28 – 7.34 (m, 2H), 7.18 – 7.24 (m, 1H), 7.15 (d, J= 13.64 Hz, 1H), 7.10 (d, J= 8.08 Hz, 2H), 4.91 (s, 2H), 3.82 (s, 3H), 3.07 (s, 3H), 2.17 (s, 3H), 2.15 (s, 3H ).Mass spectrum (m/z, +ve ion mode): 472 [M++l], 474 [M++l+2].

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; RANBAXY LABORATORIES LIMITED; VERMA, Ashwani Kumar; MALHOTRA, Sanjay; GHORPADE, Satish Madhav; DAWANGE, Mahesh Balasaheb; RAY, Abhijit; GUPTA, Suman; SRIVASTAVA, Punit; DASTIDAR, Sunanda Ghosh; WO2012/14127; (2012); A1;,
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. 1939-99-7, name is Phenylmethanesulfonyl chloride, A new synthetic method of this compound is introduced below., Computed Properties of C7H7ClO2S

Collidine (0.59 mL, 4.5 mmole) was added in one portion to a stirred solution of the compound of Example 94 (0.89 g, 3.7 mmole) and benzylsulfonyl chloride (0.86 g, 4.5 mmole) in acetonitrile (20 ml) cooled in an ice bath. The solution was stirred for 5 minutes at 0 C., followed by 45 minutes at room temperature. The reaction mixture was quenched with water, then diluted with ethyl acetate (100 mL), washed with 3% HCl (until aqueous layer was pH 1), and brine, dried over magnesium sulfate, and the solvent was removed. The residue was dissolved in methanol, concentrated to a volume of approximately 3 mL, and the product was precipitated with the addition of diethyl ether. The precipitate was filtered to give 0.67 g of the title compound. The filtrate was concentrated and chromatographed on flash silica gel using 20 to 67% ethyl acetate hexanes as eluent. An additional 0.20 g of the title compound was recovered. A total of 0.87 g of the title compound (59% yield) was recovered. Rf=0.29 (silica gel, 33% ethyl acetate/hexanes).

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; Corvas International, Inc.; US6342504; (2002); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 329944-72-1, These common heterocyclic compound, 329944-72-1, name is 3-Bromo-5-chlorotoluene, 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 1 : To a solution of 3-bromo-5~chlorotoluene (754 mg, 3,67 mmol) in diethyl ether (20 mL) was added dropwise butyllithium (1.5 mL, 3.67 mmol) at -78 C. The resulting solution was stirred at -78 C for 0.5h before addition of 3a (558 mg, 1.835 mmol) as one portion. The reaction mixture was stirred from -78 C to rt over 16h before quenching with sat. NaHCPatent; MERCK SHARP & DOHME CORP.; DING, FA-Xiang; JIANG, Jinlong; SHEN, Dong-Ming; SHEN, Hong; SHI, Zhi-Cai; WO2011/137024; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 115843-99-7, The chemical industry reduces the impact on the environment during synthesis 115843-99-7, name is 4-Bromo-3-chloro-2-fluoroaniline, I believe this compound will play a more active role in future production and life.

Anhydrous DMF (60 ml_) is added to a flask charged with bromide 9a (5.00 g, 22.2 mmol), Jb/s-(pinacolato)diborane (8.48 g, 33.4 mmol) and potassium acetate (6.35 g, 66.8 mmol) and the resulting suspension is deoxygenated by bubbling a stream of N2 gas through the mixture for 45 min. 1 ,1′-bis(diphenylphosphino)ferrocene (2.73 g, 3.34 mmol) is then added and the mixture is deoxygenated for approximately a further 5 min and is then heated to 950C. After 16 h, the dark reaction mixture is cooled, extracted with EtOAc (500 ml. and 300 ml.) and washed with 1:1 water/brine (600 mL) and brine (600 ml_). The combined extracts are dried over anhydrous MgSO4, filtered and evaporated to a black syrup which is purified by flash column chromatography (EtOAc / hexane) to afford the boronate 9b as white solid contaminated with <25 % of the diboron reagent (4.24 g, 62% 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, 4-Bromo-3-chloro-2-fluoroaniline, other downstream synthetic routes, hurry up and to see. Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GmbH; WO2009/62289; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 694-80-4, A common heterocyclic compound, 694-80-4, name is 1-Bromo-2-chlorobenzene, molecular formula is C6H4BrCl, 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.

III – 1 raw materials (0.5g, 2 . 6mmol) dissolved in 42 ml in the mixed solvent (toluene/ethanol/water, 3:1: 3, v/v/v), adding raw material III – 2 (0.3g, 2 . 6mmol), triphenyl phosphorus palladium (0.15g, 0 . 13mmol), anhydrous sodium carbonate (0.69g, 6 . 5mmol), under the protection of nitrogen, 60 C heating reaction 24h. After the reaction cooled to room temperature, water 20 ml dilution, diatomite groundwork for filtering, ethyl acetate (15 ml ¡Á 3) washing the filter cake, the filtrate with ethyl acetate (30 ml ¡Á 4) extraction, the combined organic phase to saturated NaCl solution (20 ml ¡Á 2) washing, to obtained organic phase dried with anhydrous sodium sulfate, filtered, filtrate is decompressed and evaporate the solvent, the residue by column chromatography (petroleum ether/ethyl acetate, 70:30, v/v) to obtain the gray solid 0.47g, yield 84%.

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; China Pharmaceutical University; Huang Wenlong; Qian Hai; Liu Chunxia; (26 pag.)CN106748922; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1996-30-1, name is 3-Bromo-4-fluorochlorobenzene, 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 1996-30-1, Application In Synthesis of 3-Bromo-4-fluorochlorobenzene

Step 1: [4-({(l/?,3/?,45)-3-({[ieri-Butyl(dimethyl)silyl]oxy}methyl)-4- [(triisopropylsilyl)oxy]cyclopentyl}amino)pyrimidin-5-yl]{5-chloro-4-[(S)-(5-chloro-2- fluorophenyl)(hydroxy)methyl]-2-thienyl}methanone and Butyl(dimethyl)silyl]oxy}methyl)-4-[(triisopropylsilyl)oxy]cyclopentyl}amino)pyrimidin-5-yl]{5- chloro-4-[(J?)-(5-chloro-2-fluorophenyl)(hydroxy)methyl]-2-thienyl}methanone. [00786] To a solution of 3-bromo- l -chloro-4-fluorobenzene (69.0 uL, 0.57 mmol) in THF (5.00 mL) at 0 C was added dropwise 2 M isopropylmagnesium chloride in Et20 (0.31 mL, 0.62 mmol) and the mixture was stirred at 0 C for 1 hour, and then warmed to rt overnight. This mixture was added dropwise to a solution of lnt-270 ( 185 mg, 0.28 mmol) in THF (8.0 mL) at -40 C and the reaction was allowed to stir at for 30 min at same temperature. The reaction was quenched by addition of saturated NH4C1 and extracted with EtOAc (x2). The combined organic layers were washed with brine, dried over MgS04, and concentrated in vacuo. The residue was purified by ISCO column chromatography (20% EtOAc in hexanes as eluent) to give 0.14g (63%) of the title compounds. LCMS (FA): m/z =782.2 (M+H)

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, 3-Bromo-4-fluorochlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DUFFEY, Matthew O.; ENGLAND, Dylan; FREEZE, Scott; HU, Zhigen; LANGSTON, Steven, P.; MCINTYRE, Charles; MIZUTANI, Hirotake; ONO, Koji; XU, He; (684 pag.)WO2016/4136; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 15205-11-5, These common heterocyclic compound, 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, 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.

Example 120; 2-(3-butyl-5-methyl-1 -phenyl-1 H-pyrazol-4-yl)-lambda/-[(2-chloro-4- fluorophenyl)methyl]acetamide (E120)(3-Butyl-5-methyl-1 -phenyl-1 H-pyrazol-4-yl)acetic acid (0.100 g, 0.36 mmol, prepared as described below) was dissolved in dimethylformamide (5 ml) and treated with water soluble carbodiimide (0.138 g, 0.72 mmol), 1-hydroxybenzotriazole (0.099 g, 0.72 mmol), diisopropylethylamine (0.26 ml, 1.45 mmol), and [(2-chloro-4- fluorophenyl)methyl]amine (0.1 17 g, 0.72 mmol) and the mixture was stirred at room temperature for -48 hrs. The mixture was diluted with 2M aqueous hydrogen chloride and extracted with ethyl acetate. The combined organic layers were then washed with saturated aqueous sodium hydrogen carbonate, dried over anhydrous sodium sulphate, and evaporated to give the crude product. This was purified by mass-directed automated HPLC to give the title compound as product (0.087 g) after concentration of the combined product fractions and trituration with diethyl ether. LC/MS [M+H]+ = 414, retention time = 3.21 minutes.

Statistics shows that 2-Chloro-4-fluorobenzylamine is playing an increasingly important role. we look forward to future research findings about 15205-11-5.

Reference:
Patent; GLAXO GROUP LIMITED; WO2008/138876; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, 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 210532-25-5, Quality Control of 3,5-Difluorobenzene-1-sulfonyl chloride

General procedure: To a mixture of 3-amino-2-methyl-thieno[2,3-d]pyrimidin-4(6H)-one (1.0 mmol) (8 and 9) and benzenesulfonyl chloride (1.1 mmol) in DCM (10 mL) was added dropwise pyridine (1.2 mmol) in dichloromethane (2 mL). The resulting mixture was stirred at room temperature for 12 hrs. The mixture was concentrated under reduced pressure, and theresidue was treated with water (30 mL). The aqueous mixture was neutralized by the addition of aqueous 10% HCl solution and extracted with DCM (230 mL). The organicphase was washed with aqueous saturated NH4Cl solution and brine. The organic layer was separated and dried over anhydrous MgSO4, filtered, and concentrated under reducedpressure to give the crude product, which was purified by silica gel chromatography to produce the pure corresponding compounds.

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, 3,5-Difluorobenzene-1-sulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Nie, Li Fei; Bozorov, Khurshed; Huang, Guozheng; Zhao, Jiangyu; Niu, Chao; Aisa, Haji Akber; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 193; 10; (2018); p. 656 – 667;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics