Month: March 2021

These common heterocyclic compound, 104-11-0, name is 1-(4-Chlorophenyl)-N-methylmethanamine, 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. Computed Properties of C8H10ClN

General procedure: A solution of benzylamine (386 mg, 3.14 mmol), dimethyl 2,2′-(carbonylbis(oxy))dibenzoate) (1009 mg, 3.06 mmol) in tetrahydrofuran (10 mL) was stirred at 20C for 2 hrs. The solvent of the reaction mixture was evaporated under reduced pressure to give a crude oil. The crude product was purified by columnchromatography (eluent: ethyl acetate : dichloromethane = 1 : 10) to afford methyl 2-((benzylcarbamoyl)oxy)benzoate (770 mg, 2.70 mmol, 88% yield (based on dimethyl2,2′-(carbonylbis(oxy))dibenzoate))) as white powder.

The synthetic route of 1-(4-Chlorophenyl)-N-methylmethanamine has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kurouchi, Hiroaki; Otani, Yuko; Ohwada, Tomohiko; Heterocycles; vol. 93; 2; (2016); p. 705 – 713;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 3972-56-3, 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. 3972-56-3, name is 1-tert-Butyl-4-chlorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A mixture of the aryl chloride (1 mmol), arylboronic acid (1.5 mmol), Pd(OAc)2 (0.5 molpercent), dre-NHC (0.5 molpercent), K2CO3 (1.5 mmol), in DMF:water (6 mL (1:1)) in a round bottom flask was stirred at the appropriate temperature and indicated time under an air atmosphere. The mixture was added to cold water (10 mL) and extracted with ethyl acetate (2×5 mL). The organic phase was dried with MgSO4 and filtrated through a short on silica gel column. Then volatiles were removed under reduced pressure and yields were determined by GC using undecane as an internal standard. All catalytic reactions were duplicated.

The chemical industry reduces the impact on the environment during synthesis 1-tert-Butyl-4-chlorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Article; Karaca, Emine Oezge; Akkoc, Mitat; Nawaz Tahir, Muhammad; Ar?c?, Cengiz; ?mik, Fatma; Guerbuez, Nevin; Ya?ar, Sedat; Oezdemir, ?smail; Tetrahedron Letters; vol. 58; 36; (2017); p. 3529 – 3532;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 210532-25-5, A common heterocyclic compound, 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, molecular formula is C6H3ClF2O2S, 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.

To a 25 mL round bottom flask was added 0.10 g (0.35 mmol, 1.0 eq) of JD 1001-002-10 solid, 3.2 mL THF, 0.13 g (1.05 mmol, 3.0 eq) DMAP, 0.22 g (1.05 mmol, 3.0 eq. 3,5-difluorobenzenesulfonyl chloride, the reaction was stirred at room temperature for 3 hours, and the reaction was completed by TLC (developing solvent: PE: EA = 1:1). The organic phase was washed twice with 0.5N aqueous hydrochloric acid and dried over anhydrous sodium sulfateIt was separated and purified by high pressure liquid phase (CH3CN: H2O = 60:40), and lyophilized to obtain 16 mg of JD1001-2064 product in a yield of 9%.

The synthetic route of 210532-25-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kunming Jida Pharmaceutical Co., Ltd.; Xiao Xuzhi; Zhang Poyong; Lu Faguan; Wang Zhipeng; Chen Mengran; Guo Kun; Zhou Rui; Zhang Yun; (28 pag.)CN109593061; (2019); A;,
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. 116369-24-5, name is 4-Bromo-5-chloro-2-fluoroaniline, A new synthetic method of this compound is introduced below., Product Details of 116369-24-5

4-bromo-5-chloro-2-fluoroaniline (100mg, 0.446mmol),Isobutyl-1H-pyrazole-4-boronic acid pinacol ester(223 mg, 0.891 mmol),Pd (dppf) Cl2 (163 mg, 0.223 mmol)And potassium carbonate (123 mg, 0.890 mmol) were stirred in 1,4-dioxane / water (10 mL / 2 mL)Under nitrogen atmosphere, the temperature was raised to 110 C for 1 hour under microwave irradiation.Cool to room temperature,add water,Dichloromethane extraction,dry,Purification by column chromatography gave 5-chloro-2-fluoro-4- (1-isobutyl-1H-pyrazol-4-yl) aniline(67.0 mg).

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; Shanghai Hansen Bio-pharmaceutical Technology Co., Ltd.; Jiangsu Haosen Pharmaceutical Group Co., Ltd.; Tong Chaolong; Bao Rudi; Li Yuannian; (67 pag.)CN107312005; (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 6940-78-9 as follows. COA of Formula: C4H8BrCl

Example 8; Preparation 7-CBQ by a reaction of 7-HQ with 1-bromo-4-chlorobutane in 2-propanol in Presence of potassium carbonate; A mixture of 7-hydroxy-3,4-dihydro-2(1H)-quinolinone (10 g, 0.061 mole), 1-bromo-4-chlorobutane (21.5 ml, 31.88 g, 0.183 mole, 3 eq.) and potassium carbonate (9.25 g, 0.067 mole, 1.1 eq.) in 2-propanol (50 ml) was heated under reflux for 12 hours. The hot reaction mixture was filtered, and the solvent and excess 1-bromo-4-chlorobutane were removed to dryness in vacuum. 2-Propanol (32 ml) was added to the residue thus obtained and the mixture was heated under reflux to obtain a solution. A solution of 47% aqueous sodium hydroxide was added to the hot solution to produce pH of about 10-11 and the mixture was set aside at 10-15 C. for 6 hours. A colorless precipitate was collected by filtration, washed with the cold mixture of water and 2-propanol (1:3, 15 ml) and water (25 ml) and dried under reduced pressure at 50 C. overnight to obtain 7-(4-chlorobutoxy)-3,4-dihydro-2(1H)-quinolinone (14.4 g) in 92.6% yield, having a purity of 98.4% (by HPLC).

According to the analysis of related databases, 6940-78-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Naddaka, Vladimir; Brand, Michael; Davidi, Guy; Klopfer, Eyal; Gribun, Irina; Arad, Oded; Kaspi, Joseph; US2006/79689; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 115843-99-7, These common heterocyclic compound, 115843-99-7, name is 4-Bromo-3-chloro-2-fluoroaniline, 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.

To a solution of 4-bromo-3-chloro-2-fluoro-aniline (3 g, 13.4 mmol) and HATU (10.2 g, 26.7 mmol) in DMA (30 mL) was added TEA (5.58 mL, 40.1 mmol) and 3-tert-butoxy-3-oxopropanoic acid (3.09 mL, 20.0 mmol) at RT. The mixture was stirred at 50 C for 1 h, diluted with water, and extracted with EtOAc. The organic layer was washed with brine, dried over anhydrous Na 2SO 4, filtered, and concentrated in vacuo. The residue was purified by column chromatography on silica gel (gradient elution, 30 – 70% EtOAc/hexane) to give tert-butyl 3-(4-bromo-3-chloro-2-fluoro-anilino)-3-oxo-propanoate (3.35 g).

Statistics shows that 4-Bromo-3-chloro-2-fluoroaniline is playing an increasingly important role. we look forward to future research findings about 115843-99-7.

Reference:
Patent; TAIHO PHARMACEUTICAL CO., LTD.; OTSUKA PHARMACEUTICAL CO., LTD.; SHIMAMURA, Tadashi; KATO, Ryo; MIURA, Risako; MITA, Takashi; OGAWA, Takahiro; SAGARA, Yufu; JOHNSON, Christopher Norbert; HOWARD, Steven; DAY, James Edward Harvey; ST. DENIS, Jeffrey David; LIEBESCHUETZ, John Walter; (345 pag.)WO2020/22323; (2020); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 367-22-6, These common heterocyclic compound, 367-22-6, name is 4-Chloro-3-fluoroaniline, 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 substituted anilines (4.70 mmol) in toluene (25 mL) was added to the above reaction solution, followed by stirring for 3 h. Upon completion of the reaction, the resulting mixture was cooled to 20 C.The solid thus obtained was filtered under a reduced pressure and washed with toluene (20 mL). Isopropanol (18 mL) was added to thesolid, which was then stirred for 5 h. The resulting solid was filtered and washed with isopropanol (10 mL). The solid was dried at 50 C in the oven to afford 3a-f as white powder.

Statistics shows that 4-Chloro-3-fluoroaniline is playing an increasingly important role. we look forward to future research findings about 367-22-6.

Reference:
Article; Cai, Zhi-Qiang; Jin, Zheng-Sheng; Zheng, De-Qiang; Hou, Ling; Huang, Guan-Wang; Tian, Jun-Qiang; Wang, Guo-Jiang; Journal of Chemical Research; vol. 40; 9; (2016); p. 573 – 575;,
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. 102-49-8, name is 3,4-Dichlorobenzylamine, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H7Cl2N

General procedure: Compounds 1?6 were prepared according to conventional organic synthesis methods. 3-Chloropyrazine-2-carboxamide (1.27 mmol) was dissolved in THF (20 mL) in a round bottom flask and after that treated with two equivalents of the corresponding benzylamine and an equimolar amount of triethylamine. The reaction was conducted with continuous stirring and heating (70 ¡ãC) under reflux in an oil bath for 15 h. Compounds 7?15 were synthesised using a microwave reactor with a focused field. 3-Chloropyrazine-2-carboxamide (1.27 mmol) was put into a thick-walled tube together with the corresponding benzylamine (2.54 mmol), pyridine (1.27 mmol), methanol (approx. 5 mL) and a magnetic stir bar and then sealed with a special cap. The reaction parameters were set according to the previously published paper as follows?140 ¡ãC, 30 min, 200 W [29]. Reaction progress was checked by TLC (hexane:ethyl acetate?1:1). Regardless of the synthesis method used,all reaction mixtures were adsorbed on silica and subjected to preparative flash chromatography (hexane and ethyl acetate, gradient elution, detection wavelengths 260 nm and 280 nm). Products were recrystallized from ethanol or ethanol and water if necessary. All final substances were chemically characterized (1H-NMR, 13C-NMR, IR, melting point and elemental analysis).

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:
Article; Jandourek, Ondrej; Tauchman, Marek; Paterova, Pavla; Konecna, Klara; Navratilova, Lucie; Kubicek, Vladimir; Holas, Ondrej; Zitko, Jan; Dolezal, Martin; Molecules; vol. 22; 2; (2017);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 26487-67-2,Some common heterocyclic compound, 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, molecular formula is C8H17Cl2N, 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 solution of 1,1-bis(4-hydroxyphenyl)-2-phenylpent-1-ene (32.6 mg, 98.7 mumol) in DMF (0.99 mL) at 0 ¡ãC was added 60percent sodium hydride (dispersion in paraffin liquid, 31.6 mg, 0.790 mmol). The reaction mixture was stirred for 10 min at 50 ¡ãC and then N-(2-chloroethyl)hexahydro-1H-azepine hydrochloride (64.5 mg, 0.326 mmol) was added in portions at room temperature. After the reaction mixture had been stirred for 3.5 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*12 (compound 11) (42.8 mg, 75percent) as a white solid

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;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 67120-39-2, A common heterocyclic compound, 67120-39-2, name is 5-Chloro-2,3-dihydro-1H-inden-1-amine, molecular formula is C9H10ClN, 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.

A mixture of compound 1 (110 mg, 0.302 mmol), crude 5-chloro-l- indanamine (100 mg, 0.604 mmol), and potassium carbonate (167 mg, 1.24 mmol) in dioxane (15 mL) was refluxed for 2 hrs. The volatiles were removed in vacuo. The residue was partitioned into ethyl acetate and water. The organic extracts were dried over anhydrous sodium sulfate and concentrated in vacuo. The crude product was purified by preparative- HPLC to give 32 mg (21% yield) of compound A7 as a white solid: 91.2% purity (LCMS); MS m/z: 498.2 (M+l); 1H NMR (CDC13, 500 MHz) delta 8.43 (d, J= 8.5 Hz, 1H), 7.90 (t, J = 8.0 Hz, 1H), 7.66 (t, JHF = 53.5 Hz, 1H), 7.47-7.38 (m, 2H), 7.33-7.25 (m, 2H), 7.24-7.19 (m, 1H), 5.64 (m, 1H), 5.51 and 5.44 (2d, J= 8.5 and 8.5 Hz, 1H), 3.93 (m, 4H), 3.82 (m, 4H), 3.05 (m, 1H), 2.95 (m, 1H), 2.75 (m, 1H), 2.03 (m, 1H) 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; PATHWAY THERAPEUTICS INC.; BROWN, David, S.; MATTHEWS, David, J.; WO2012/135166; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics