Month: September 2021

Related Products of 766545-20-4, 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 766545-20-4 as follows.

To a solution of 2-chloro-5,6,7,8-tetrahydro-l,6-naphthyridine hydrochloride (available from Activate Scientific) (3.0 g, 15 mmol) in DCM (50 mL) was added NEt3 (4.44 g, 6.1 mL, 44 mmol). After 15 min, methylchloroformate (2.1 g, 1.7 mL, 22 mL) was added and the resulting mixture stirred at RT for 16 h. The reaction was diluted with DCM, washed with saturated NaHCO3 (aq.), then brine, dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by FCC (SiO2, eluting with 2:1 heptane / EtOAc) to give the title compound (3.17 g, 96%) as white solid.LCMS data: Calculated MH+ (227); Found 100% (MH+) m/z 227, Rt = 1.11 (2 min method). 1H NMR (500 MHz, CHLOROFORM-J) delta ppm 7.38 (1 H, br. s.), 7.18 (1 H, d, J=8.1 Hz), 4.62 (2 H, br. s.), 3.78 – 3.83 (2 H, m), 3.72 (3 H, s), 3.00 (2 H, t, J=5.3 Hz).

According to the analysis of related databases, 766545-20-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; EVOTEC NEUROSCIENCES GMBH; WO2009/121812; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 699-89-8, name is 4,7-Dichlorothieno[2,3-d]pyridazine, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 4,7-Dichlorothieno[2,3-d]pyridazine

One equivalent of dichloride (1) and 2.2 equivalent of M-NH2 are refluxed in an appropriate amount of n-butanol at 150C for 10 hrs. The reaction mixture is allowed to cool to room temperature and the precipitate (4) that forms is filtered and washed sequentially with isopropyl alcohol, 4.0 N KOH, H2O, and hexane, and then dried. The crude product (4) is purified by preparative TLC or flash chromatography on silica gel using dichloromethane/methanol (95:5) as the eluent. Final product is confirmed by LC/MS and/or NMR. The invention compounds of Examples 26 – 33 and 75 as shown in the below table were prepared by method A-2.

According to the analysis of related databases, 699-89-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BAYER CORPORATION; EP1228063; (2009); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 108-70-3, name is 1,3,5-Trichlorobenzene, molecular formula is C6H3Cl3, 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. Recommanded Product: 1,3,5-Trichlorobenzene

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.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 108-70-3, its application will become more common.

Reference:
Article; Reimann, Sebastian; Ehlers, Peter; Sharif, Muhammad; Spannenberg, Anke; Langer, Peter; Tetrahedron; vol. 72; 8; (2016); p. 1083 – 1094;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 3386-33-2,Some common heterocyclic compound, 3386-33-2, name is 1-Chlorooctadecane, molecular formula is C18H37Cl, 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.

After dropping 173.4 g (0.6 mol) of 1-chlorooctadecane thereinto within about 15 minutes, the mixture was allowed to stand overnight under stirring at room temperature. Then the reaction mixture was washed with 500 ml of isopropyl ether and thus crystals of acryloyloxyethyl-N,N-dimethyloctadecylammonium chloride were obtained.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Chlorooctadecane, its application will become more common.

Reference:
Patent; Hisamitsu Pharmaceutical Co, Inc.; US5665348; (1997); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 1940-29-0, 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. 1940-29-0 name is 4-Bromo-3,5-dichloroaniline, 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.

(4-Bromo-3,5-dichloro-phenyl)-[5-methanesulfonyl-2-(4-methoxy-benzyl)-2H- [l,2,4]triazol-3-yl]-amine In a 25 mL round bottle, 5-chloro-l-(4-methoxybenzyl)-3-(methylsulfonyl)-lH-l,2,4-triazole (200 mg, 663 muiotaetaomicron, Eq: 1.00) was combined with DMF (3 mL) to give a colorless solution. 4- Bromo-3,5-dichloroaniline (160 mg, 663 muiotaetaomicron, Eq: 1.00) and sodium 2-methylpropan-2-olate (127 mg, 1.33 mmol, Eq: 2.00) were added. The reaction was degassed by nitrogen for 5 min. The resulting solution was heated to 85 C overnight under nitrogen. The reaction mixture was cooled and diluted with 20 mL H20, added Ether (30×2 mL) to extract the product, dried the organic layer over anhydrous Na2S04, concentrate the solution, purify the compound by column (Hexanes/EtOAc = 70/30) to afford the compound 180mg (54%). MH+ 507.0

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-3,5-dichloroaniline, and friends who are interested can also refer to it.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; DING, Qingjie; JIANG, Nan; WEIKERT, Robert James; WO2014/135472; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 64628-73-5, name is 3-Chloro-4-(trifluoromethoxy)aniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 64628-73-5

An ice-cold mixture of 98% H2SO4 (0.75 mL) and water (2.25 mL) was added to 3-chloro-4-(trifluoromethoxy)aniline (53) (1 .00 g, 4.73 mmol) and the resulting salt was crushed (using a glass rod) and cooled in an ice bath. A solution Of NaNO2 (359 mg, 5.20 mmol) in cold water (0.75 mL, then 0.25 mL) was added drop-wise, and the mixture was stirred at 0 0C for 12 min. A solution of urea (42.6 mg, 0.709 mmol) in cold water (0.25 mL) was added, and the mixture was stirred at 0 0C for 3 min. Finally, a solution of KI (1.65 g, 9.94 mmol) in cold water (1.6 mL, then 0.2 mL) was added slowly, and the mixture was stirred at room temperature for 10 min, and then at 52 C for 2 h. The resulting cooled mixture was diluted with ice-water (45 mL) and extracted with CH2Cl2 (4x 50 mL). The extracts were sequentially washed with an aqueous solution of Na2SO3 (30 mL of 0.5%) and then with water (40 mL) and finally concentrated carefully under reduced pressure at 17 C. The resulting oil was chromatographed on silica gel, eluting with pentane, to give 2-chloro-4-iodo- 1 -(trifluoromethoxy)benzene (54) (1.24 g, 81%) as a colourless oil (a white solid on freezing); 1H NMR (CDCl3) delta 7.82 (d, J = 2.1 Hz, 1 H), 7.61 (dd, J = 8.6, 2.1 Hz, 1 H), 7.05 (dq, J = 8.6, 2.0 Hz, 1 H); HRAPCIMS calcd for C7H3ClF3IO mlz (M+) 323.8834, 321.8864, found 323.8834, 321.8861.

The synthetic route of 64628-73-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLOBAL ALLIANCE FOR TB DRUG DEVELOPMENT; DENNY, William, Alexander; THOMPSON, Andrew, M.; BLASER, Adrian; MA, Zhenkun; PALMER, Brian, Desmond; SUTHERLAND, Hamish, Scott; KMENTOVA, Iveta; WO2011/14774; (2011); 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. 95-81-8, name is 2-Chloro-5-methylaniline, A new synthetic method of this compound is introduced below., COA of Formula: C7H8ClN

(A-82-21) tert-Butyl 4-(2-chloro-5-methylphenylcarbamoyl)-3-[4-cyclopropyl-5-(3-isobutylcyclobutyl)isoxazol-3-yl]butanoate Mono-tert-butyl 3-[4-cyclopropyl-5-(3-isobutylcyclobutyl)isoxazol-3-yl]glutarate (2.83 g) and DMF (28 mL) were mixed. After an addition of 2-chloro-5-methylphenylamine (1.184 g), HOBt.H2O (1.28 g) and WSC.HCl (1.60 g) to the resultant solution, the mixture was stirred at RT for 2 days. To the reaction mixture was added saturated aqueous sodium bicarbonate, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium bicarbonate, water and brine, then dried over sodium sulfate. The sodium sulfate was filtered off and the filtrate was concentrated in vacuo. The resultant residue was purified by silica gel column chromatography (Eluent: ethyl acetate/hexane=1/15?1/10?1/8) to give the title compound (1.241 g).

The synthetic route of 95-81-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JAPAN TOBACCO INC.; US2012/322837; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 1005-56-7, name is O-Phenyl carbonochloridothioate, molecular formula is C7H5ClOS, 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. Product Details of 1005-56-7

6a (100 mg, 0.30 mmol) was dissolved in 5 mL of acetonitrile,4-Dimethylaminopyridine (162 mg,1.33 mmol) andPhenylchloroformate (0.1 mL)After stirring at 0-60 C for 2-12 hours, the reaction solution was filtered, concentrated and separated by column(N-hexane / ethyl acetate: 20/1) gave a colorless oil 8 (128 mg, 0.27 mmol, 90%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1005-56-7, its application will become more common.

Reference:
Patent; China Pharmaceutical University; Xie Weijia; Zhang Chenxi; Wang Zihao; Wu Xiaoming; Xu Jinyi; Yao Hequan; Lin Aijun; (12 pag.)CN107043403; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 918538-05-3, 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. 918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Compound 183a was prepared from tert-butyl 2,4-dichloro-5,6-dihydropyrido[3,4- d]pyrimidine-7(8H)-carboxylate (182a) (1.0 g, 3.29 mmol) in 2-Propanol (15 mL) using DIPEA (2.3 mL, 13.15 mmol) and 1-(3,4,5-trimethoxyphenyl)-1H-imidazol-4-amine (57a) (0.98 g, 3.95 mmol). This gave after workup and purification by flash column chromatography [silica gel, (12 g) eluting with DMA-80 in DCM (0 to 80%)] fert-butyl 2-chloro-4-((l-(3,4,5- trimethoxyphenyl)-lH-imidazol-4-yl)amino)-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)- carboxylate (183a) (0.87 g, 51 % yield) as a buff solid; NMR (300 MHz, DMSO-^e) delta 9.65 (s, 1H, D20 exchangeable), 8.16 (d, J = 1.5 Hz, 1H), 7.78 (d, J = 1.6 Hz, 1H), 6.90 (s, 2H), 4.35 (s, 2H), 3.87 (s, 6H), 3.69 (s, 3H), 3.61 (t, J = 5.8 Hz, 2H), 2.69 – 2.60 (m, 2H), 1.43 (s, 9H).

The synthetic route of 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOCRYST PHARMACEUTICALS, INC.; KOTIAN, Pravin, L.; BABU, Yarlagadda, S.; KUMAR, V., Satish; ZHANG, Weihe; LU, Peng-Cheng; RAMAN, Krishnan; (747 pag.)WO2018/232094; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 698-01-1, 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. 698-01-1 name is 2-Chloro-N,N-dimethylaniline, 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.

General procedure: A mixture of benzoyl chloride 1a (0.5 mmol), N,N-dimethylaniline 2a (1.5 mmol), KMnO4 (1.5 equiv.) and CH3CN (2.0 mL) was placed in a 25 mL reaction straight tube under air atmosphere. The tube was then placed in an oil bath, stirred and heated at 60 C for 6 h. After cooling to room temperature, the system was flushed to Sand core funnel using dichloroethane (rinsing three times, VDCM < 50 mL), Vacuum filtration, and the volatile solvent was removed in vacuo. The crude product was purified through a silica gel column (ethyl acetate/petroleum ether = 1:5) to afford (93%) a yellow liquid. At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-N,N-dimethylaniline, and friends who are interested can also refer to it. Reference:
Article; Zhang, Zhang; Liu, Yong-Hong; Zhang, Xi; Wang, Xi-Cun; Tetrahedron; vol. 75; 19; (2019); p. 2763 – 2770;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics