Category: chlorides-buliding-blocks

Related Products of 2533-69-9, A common heterocyclic compound, 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, molecular formula is C3H4Cl3NO, 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. Synthesis of 3-(4-chloro-3-fluorophenyl)-2-(trichloromethyl)-3H-imidazo[4,5-b]pyridine (C20) Methyl 2,2,2-trichloroethanimidoate (0.743 mL, 6.00 mmol) was added to a solution of N2-(4-chloro-3-fluorophenyl)pyridine-2,3-diamine (C12) (951 mg, 4.00 mmol) in acetic acid (4 mL), and the reaction mixture was stirred at room temperature for 5 hours. After concentration in vacuo, the residue was purified via chromatography on silica gel (Gradient: 5% to 100% ethyl acetate in heptane) to afford the product as a white solid. Yield: 1.04 g, 2.85 mmol, 71%. LCMS m/z 366.0 [M+H]+. 1H NMR (400 MHz, CDCl3) delta 8.49 (dd, J=4.7, 1.5 Hz, 1H), 8.27 (dd, J=8.1, 1.5 Hz, 1H), 7.64 (ddd, J=8.5, 7.8, 0.3 Hz, 1H), 7.42 (dd, J=8.1, 4.7 Hz, 1H), 7.39 (ddd, J=8.8, 2.4, 0.2 Hz, 1H), 7.32 (ddd, J=8.5, 2.4, 1.3 Hz, 1H).

The synthetic route of 2533-69-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chappie, Thomas Allen; Verhoest, Patrick Robert; Patel, Nandini Chaturbhai; Hayward, Matthew Merrill; US2014/235612; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 33050-38-3, A common heterocyclic compound, 33050-38-3, name is 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine, molecular formula is C5H2Cl2N4, 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.

b) The 3-chloro-6-(morpholin-4-yl)[1,2,4]triazolo[4,3-b]pyridazine can be prepared in the following way:0.9 cm3 of morpholine and 1.4 cm3 of triethylamine are added to a solution of 1.89 g of commercial 3,6-dichloro[1,2,4]triazolo[4,3-b]pyridazine in 20 cm3 of N,N-dimethylformamide. The reaction is stirred at 20 C. for 19 1H). 60 cm3 of water are added and the mixture is extracted with ethyl acetate. The organic phase is washed with water and with brine and then dried over magnesium sulphate and concentrated to dryness, to give a beige solid. The latter is chromatographed by solid deposit on a Merck cartridge of 70 g of silica 15-40 mum, elution being carried out with a gradient of 100% dichloromethane to 95/5 dichloromethane/methanol. 1.97 g of 3-chloro-6-(morpholin-4-yl)[1,2,4]triazolo[4,3-b]pyridazine are obtained in the form of a very pale yellow solid, the characteristics of which are as follows:MASS SPECTRUM: UPLC-MS-DAD-ELSD: 240=MH+.

The synthetic route of 33050-38-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; sanofi-aventis; US2010/298315; (2010); 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. 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, A new synthetic method of this compound is introduced below., Quality Control of 2,2,2-Trifluoro-N-phenylacetimidoyl chloride

1.46 g (1.45 mmol) VIII and 0.93 g (4.5 mmol)2,2,2-Trifluoro-N-phenyliminoacetyl chloride is dissolved in 30 mL of acetone,0.62 g (4.5 mmol) of potassium carbonate was added in portions and allowed to react at room temperature overnight.TLC (PE: EA = 2:1) was monitored and the reaction was completed.The reaction was quenched with 0.2 mL of methanol, filtered, and the filtrate was dried.Column chromatography (PE: EA = 4:1) gave 1.7 g of VI white solid, yield 99%.

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 Pharmaceutical Industry Institute; China Pharmaceutical Industry Zongyuan; Zhang Hongliang; Wang Zhefeng; Yi Bing; Wang Shengli; Liang Qian; Li Changsheng; (18 pag.)CN108299523; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 2533-69-9, 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.

2.00 g (12.0 mmol) Methyl-3,4-diamino-benzoate were dissolved in 50 ml concentrated acetic acid. Then 2.09 ml (1.4 equiv.) methyl-2,2,2-trichloroacetimidate were added slowly and the resulting mixture was stirred at room temperature for 2 h. The mixture was diluted with 100 ml toluene and the solvent was removed under reduced pressure. The residue was taken up in dichloromethane and washed once with a saturated NaHCO3-solution and once with brine. The organic layer was dried over MgSO4 and the solvent was removed under reduced pressure to give pure methyl-2-trichloromethyl-1H-benzoimidazole-5-carboxylate as a light brown amorphous solid. Yield: 3.64 g MS (ES+): m/e = 293, chloro pattern.

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; Aventis Pharma Deutschland GmbH; EP1479676; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 19230-27-4,Some common heterocyclic compound, 19230-27-4, name is 1,3-Dibromo-2-chlorobenzene, molecular formula is C6H3Br2Cl, 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 suspension of I ,3 dibromo2chorobenzene (300 mg, 1.11 mmo), 4methoxypiperidine (168 mg, 1.11mmo), sodium tert-butoxide (160 mg, 167 mmo) in touene (30 m), was added BNAP (35 mg, 005 mrnofl and Pd2(dba)3 (20 mg, 002 mmo) at once. The mixture was degassed with nitrogen for 10 minutes and then heated at 140 C for I h in microwave. After coohng to rt, the reaction mixture was diuted with water and extracted with EtOAc(x 3). The combined organic extracts were dried (Na2SO4), fi[tered and concentrated. Purification (FCC, Si02 0 -. 100% EtOAc/hexanes) afforded the tWe compound as a oH (168 mg, 50% yied). MS (ES): mass cacd. for C12H15BrCNO, 304.6; mfz found, 305.6 [M+HJ. 1H NMR (400 MHz, DMSO): oe 742 (dd, J= 7.7, 1.7 Hz, IH), 7.28-7.14 (m, 2H), 3.39-3.33 (m, IH), 3.28 (s, 3H), 3.14(dt, J= 10.5, 4.5 Hz, 2H), 277 (ddd, J=12.0, 9.2, 3.0 Hz, 2H), 2.04- 1.91 (m, 2H), 1.61 (dtd, J= 12.2, 8.8, 3.4 Hz, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Dibromo-2-chlorobenzene, its application will become more common.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; RAVULA, Suchitra; SWANSON, Devin M.; SAVALL, Bradley M.; AMERIKS, Michael K.; (250 pag.)WO2016/176449; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 220227-21-4, name is 2,4,5-Trifluorobenzene-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 220227-21-4, Formula: C6H2ClF3O2S

A mixture of 2,4,5-trifluorobenzene-1-sulfonyl chloride (5.00 g, 21.7 mmol), 2,4- dimethoxybenzylamine (3.63 g, 21.7 mmol), diethylpropylethylamine (3.36 g, 26.0 mmol) in dichloromethane (100 mL) was stirred at ambient temperature for 16 h. The mixture was diluted in dichloromethane (100 mL), washed with iN hydrochloric acid, 25% aqueous ammonium chloride and brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo and the residue was crystallized from dichloromethane/hexanes to obtain N-(2,4-dimethoxybenzyl)-2,4,5- trifluorobenzenesulfonamide as a cream solid in 95% yield (7.5 g): 1H NMR (300 MHz, CDCI3) delta 7.55-7.47 (m, 1H), 6.81-6.76 (m, 2H), 6.25-6.20 (m, 2H), 5.50 (s, 1H), 4.18 (5, 2H), 3.76-3.73 (m, 6H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,4,5-Trifluorobenzene-1-sulfonyl chloride, and friends who are interested can also refer to it.

Reference:
Patent; XENON PHARMACEUTICALS INC.; SUN, Shaoyi; ZENOVA, Alla, Yurevna; CHAFEEV, Mikhail; JIA, Qi; ZHANG, Zaihui; OBALLA, Renata, Marcella; WO2013/64983; (2013); 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. 7464-11-1, name is 5,7-Dichloro-2-methylthiazolo[5,4-d]pyrimidine, A new synthetic method of this compound is introduced below., Quality Control of 5,7-Dichloro-2-methylthiazolo[5,4-d]pyrimidine

Into a 50 mL round-bottom flask, was placed a solution of intermediate 38.2 (121 mg, 0.58 mmol, 1.05 equiv) in CH3CN (10 mL),compound 23.1 (121 mg, 0.55 mmol, 1.00 equiv) and K3P04 (352 mg, 1.66 mmol, 3.00 equiv). The reaction was stirred overnight at 80 C. The solids were filtered out and the resulting solution was concentrated under vacuum. The crude was purified using flash column chromatography to give 140 mg (65%) of intermediate 38.3 as a white solid.

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; NIMBUS IRIS, INC.; ROMERO, Donna L.; MASSE, Craig E.; ROBINSON, Shaughnessy; GREENWOOD, Jeremy Robert; HARRIMAN, Geraldine; WO2015/48281; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 41965-95-1, name is 3-Chloro-4-methoxybenzylamine Hydrochloride, 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. Product Details of 41965-95-1

To a 25 ml three-necked flask was added ethyl 2,4-dichloro-5-pyrimidinecarboxylate (150 mg, 0.679 mmol)Triethylamine (270 mg, 2.668 mmol), dichloromethane (2 ml), gradually stirred to dissolve,The ice bath was cooled to 0 C or below, and 3-chloro-4-methoxybenzylamine hydrochloride (145 mg, 0.697 mmol) was added in portions to the reaction solution, and the reaction was carried out for two hours after completion of the addition.L-proline (105 mg, 1.038 mmol) was added dropwise to the reaction solution, and the reaction was continued for 2 hours.The reaction solution was added to water (30 ml) and extracted with dichloromethane.The organic phases were combined, washed twice, dried over anhydrous sodium sulfate, the desiccant was filtered off, and the organic phase was concentrated to the crude product.The crude product was purified by silica gel column chromatography (petroleum ether: ethyl acetate = 6: 1) to give 200 mg of product in 70% yield.

The synthetic route of 3-Chloro-4-methoxybenzylamine Hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUZHOU WANGSHAN WANGSHUI BIOMEDICAL CO LTD; TOPHARMAN SHANGHAI CO LTD; SHANDONG TOPHARMAN PHARMACEUTICAL CO LTD; TIAN, GUANGHUI; LI, JUNQI; (17 pag.)CN104650045; (2017); B;,
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. 697-86-9, name is 2-Bromo-4,6-dichloroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 697-86-9

1. 2,3,5-Trichlorobromobenzene Sodium nitrite (3.88 g, 0.056 mole) was added in portions to concentrated sulphuric acid (28.16 ml) stirred below 10 C. A solution of 2-bromo-4,6-dichloroaniline (12 g, 0.05 mole, Lancaster) in glacial acetic acid (126 ml) was added maintaining the temperature below 10 C. The mixture was stirred below 10 C. for 1 hr and then slowly added to a stirred solution of cuprous chloride (10.11 g, 0.10 mole) in concentrated hydrochloric acid (101.05 ml) at room temperature. The mixture was then stirred at room temperature for 17 hrs. The product was filtered, washed with water (3*50 ml), dissolved in chloroform (150 ml), dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated in vacuo to give the desired product. Yield 10 g (77%), M.p. 55-57 C.

The synthetic route of 697-86-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Glaxo Wellcome, Inc.; US6255307; (2001); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 14752-66-0,Some common heterocyclic compound, 14752-66-0, name is Sodium 4-chlorobenzenesulfinate, molecular formula is C6H4ClNaO2S, 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: I2 (0.5 mmol) was added to a solution of alkynes (0.5 mmol),sodium benzenesulfnates (1.0 mmol) and DTBP (1.0 mmol)in C2H5OH: H2O (2 mL:2 mL), and the reaction mixture wasstirred and heated at 60C for 2.0 h. Then, the mixture wascooled to room temperature, quenched by Na2S2O3, dilutedwithwaterandextractedbyCH2Cl2 (10mL ×3).Thecombined organic layer was washed with water and dried over anhydrousNa2SO4. The solvent was removed in vacuum and the targetcompound was obtained by column chromatography on silicagel (petroleum ether: ethyl acetate = 15: 1, v: v).

The synthetic route of 14752-66-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bi, Wenzhu; Ren, Chunyan; Jia, Linguo; Xia, Xiaoyi; Chen, Xi; Chen, Xiaolan; Zhao, Yufen; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 192; 4; (2017); p. 391 – 396;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics