Month: July 2021

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. 627-42-9, name is 2-Methoxyethyl chloride, A new synthetic method of this compound is introduced below., name: 2-Methoxyethyl chloride

2,5-Di-tert-butylhydroquinone (0.2 mmol) was dissolved in anhydrous THF (20 ml). Sodium hydride (0.6 mmol) and 2-chloroethylethylether (0.4 mmol) was then added to the solution. The reaction mixture was then stirred at room temperature overnight. After removal of the solvent, the residue was partitioned between dichloromethane and aqueous NaHCO3 (0.1M). The organic portion was separated and dried over Na2SO4. After solvent removal in vacuo, the crude product was chromatographed (silica, hexanes/DCM from 5:1 to 1:1) to afford 1,4-bis(2-methoxyethoxy)-2,5-di-tert-butyl-benzene in an 81% yield. The product was characterized by 1H NMR (300 MHz, CDCl3, delta/ppm): 7.14 (s, 2H), 4.11 (t, J=4.5 Hz, 4H), 3.80 (t, J=4.5 Hz, 4H), 3.45 (s, 6H), 1.37 (s, 18H).

The synthetic route of 627-42-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhang, Zhengcheng; Zhang, Lu; Amine, Khalil; US2011/294003; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 139512-70-2, 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. 139512-70-2 name is 4-Chloro-5-fluorobenzene-1,2-diamine, 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-Chloro-5-fluoro-benzene-1,2-diamine (5.20 g; 32.4 mmoles) and 3,3,3-trifluoro-2-hydroxy-propionic acid (7.00 g; 48.6 mmoles) were suspended in 6N HCl (9 mL; 54 mmoles) under a nitrogen atmosphere. The reaction was stirred vigorously and heated to 108C for 18 hrs, then cooled to room temperature. The reaction was diluted with water (100 mL) and with ethyl acetate (100 mL), then sodium bicarbonate (6.90 g; 81.00 mmoles) was added slowly and in portions to quench the reaction. The aqueous layer was separated and extracted with ethyl acetate (3×40 mL). The extracts were combined, washed with water (30 mL) and brine (30 mL), then dried over Na2SO4. The filtrate was concentrated in vacuo to yield a crude brown solid which was then purified by column chromatography (SiO2; 30% ethyl acetate/CH2Cl2) to yield the title compound as an off-white solid. 1H NMR (400 MHz, CD3CN) delta 7.74 (d, J = 6.7 Hz, 1 H), delta 7.49 (d, J =9.5,1 H), delta 5.41 (q, J = 6.8 Hz, 1 H), delta 5.16 (br s, 1 H), delta 2.35 (s, 6H) MS calculated for C9H5ClF4N2O: 268.00 MS measured: 269 (M+H); 267 (M-H).

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

Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; WO2006/39243; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 51572-93-1, name is O-(2,4-Dichlorobenzyl)hydroxylamine hydrochloride, 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 51572-93-1, Recommanded Product: 51572-93-1

General procedure: A mixture of substituted O-benzylhydroxylamine hydrochloride (1 equiv), TEA (1 equiv) and substituted salicylaldehyde (1 equiv) was dissolved in absolute ethanol and stirred for 0.5 h. The reaction was monitored by TLC. The precipitate was filtered and recrystallized from ethanol to gain salicylaldoxime (compounds 1g-20g).

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, O-(2,4-Dichlorobenzyl)hydroxylamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zhao, Ting-Ting; Lu, Xiang; Yang, Xian-Hui; Wang, Li-Ming; Li, Xi; Wang, Zhong-Chang; Gong, Hai-Bin; Zhu, Hai-Liang; Bioorganic and Medicinal Chemistry; vol. 20; 10; (2012); p. 3233 – 3241;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 33050-38-3, These common heterocyclic compound, 33050-38-3, name is 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine, 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[1,2,4]triazolo[4,3-b]pyridazin-6-amine can be prepared in the following way:A mixture of 190 mg of commercial 3,6-dichloro[1,2,4]triazolo[4,3-b]pyridazine and 1 cm3 of aqueous ammonia at 35% in 1 cm3 of dioxane, in a sealed tube, is heated at between 70 C. and 90 C. for 3 1H). The precipitate formed is filtered off, to give 156.4 mg of 3-chloro[1,2,4]triazolo[4,3-b]pyridazin-6-amine in the form of a beige powder, the characteristics of which are as follows:MASS SPECTRUM: UPLC-MS-DAD-ELSD: 168=MH-; 170=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

Application 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.

General procedure: Preparation of 2-methyl-6-nitro-2H-indazole (5d). To a stirred mixture of 6-nitro-1H-indazole (1.0 g, 0.0061 mmol) in dichloromethane (25.0 mL) was added trifluoromethanesulfonic acid (0.54 mL, 0.0061 mmol), stirred for 5-10 min at 25-35 C. To this mixture was added methyl 2,2,2,-trichlroacetimidate (2.69 g, 0.015 mmol) at room temperature. The reaction mixture was stirred at room temperature for 16-18 h under N2. After reaction completion, chilled saturated NaHCO3 solution was added. The aqueous and organic phases were separated. Aqueous phase was extracted with dichloromethane 10 mL. Combined organic layers were washed with DM water (2 × 10 mL). Organic layer was dried over anhydrous Na2SO4, filtered, and evaporated completely under vacuum to obtain 2-methyl-6-nitro-2H-indazole (1.03 g, 95.0%) as a yellow solid.

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

Reference:
Article; Baddam, Sudhakar Reddy; Uday Kumar; Panasa Reddy; Bandichhor, Rakeshwar; Tetrahedron Letters; vol. 54; 13; (2013); p. 1661 – 1663;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 60633-25-2, 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. 60633-25-2 name is 2-Bromo-4-chloro-1-methoxybenzene, 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.

Palladium acetate(21mg, 7mol%) was added to a solution of 2-bromo-4-chloroanisole(300mg, 1.4mmol), styrene(211mg, 2mmol), triethylamine(13 muL, 0.1mmol) and triphenylphosphine(50mg, 1.9mmol) in acetonitrile(6mL), and the mixture was refluxed for 8 hours under argon atmosphere. After the reaction mixture was cooled to room temperature, the solvent was concentrated under reduced pressure and the obtained residue was diluted with ethyl acetate(15mL). After the solution was washed successively with 2N hydrochloric acid, water and brine, dried over anhydrous sodium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was purified by column chromatography on silica gel(n-hexane:ethyl acetate=10:1) to give the title compound(118mg, 35.6%) as a white powder.1H-NMR(CDCl3):d 3.85(3H, s), 6.80(1H, d, J=8.8Hz), 7.08(1H, d, J=16.8Hz), 7.17(1H, dd, J=8.8, 2.5Hz), 7.20-7.42(4H, m), 7.51-7.55(3H, m).

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

Reference:
Patent; Institute of Medicinal Molecular Design, Inc.; EP1510207; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 1939-99-7,Some common heterocyclic compound, 1939-99-7, name is Phenylmethanesulfonyl chloride, molecular formula is C7H7ClO2S, 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.

4. 3-Benzylsulfonylamino-6-methyl-1-(tert-butoxycarbonylmethyl)-2-pyridinone To a solution of 3-amino-6-methyl-1-(tert-butoxycarbonylmethyl)-2-pyridinone (960 mg, 4.0 mmol), as prepared in the preceding step, and N-methylmorpholine (840 muL, 8.0 mmol) in methylene chloride (40 mL) was added alpha-toluenesulfonyl chloride (765 mg, 4.0 mmol) at 0 C. The reaction mixture was stirred at 0 C. for 1 h. Additional methylene chloride (50 mL) was added. The resulting methylene chloride solution was washed with saturated NaHCO3 (2*50 mL), 10% citric acid (3*50 mL) and brine (50 mL), and dried over Na2 SO4. The solvent was concentrated to give a solid which was washed with ethyl acetate/hexane (1:2, 60 mL) to give the title compound as a white solid (1.4 g, 89%). 1H-NMR (300 MHz, CDCl3) delta7.35 (d, J=7.5 Hz, 1H), 7.31 (m, 5H), 7.20 (s, 1H), 6.02 (d, J=7.4 Hz, 1H), 4.75 (s, 2H), 4.31 (s, 2H), 2.27 (s, 3H), 1.51 (s, 9H).

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

Reference:
Patent; 3-Dimensional Pharmaceuticals, Inc.; US6037356; (2000); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 118-69-4, 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. 118-69-4 name is 2,6-Dichlorotoluene, 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.

235.0 g (3.0 mol) of acetyl chloride were added dropwise with stirring at 100 C. over a period of 2 hours to a solution of 502.0 g (3.12 mol) of 2,6-dichlorotoluene and 408.0 g (3.06 mol) of aluminum trichloride. After the reaction mixture had been stirred for 2 hours at 100-105 C., it was cooled and poured into 3 l of ice and 1 l of water. The solid which precipitated in the process was filtered off with suction and washed to neutrality with water. After drying at 40 C., 500.0 g of 2,4-dichloro-3-methylacetophenone were obtained as the crude product, and this was subsequently distilled under high vacuum. (B.p.: 121-128 C. (4 mbar))

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,6-Dichlorotoluene, and friends who are interested can also refer to it.

Reference:
Patent; BASF Aktiengesellschaft; US6372693; (2002); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2106-04-9, name is 3-Chloro-2-fluoroaniline, 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 2106-04-9, SDS of cas: 2106-04-9

A round bottom flask was charged with 1 eq of 3-chloro-2-fluoroaniline (3A), 1- methyl-2-pyrrolidinone (about 1.5 M 3 A in NMP), 2.2 eq of sodium cyanide, and 1.35 eq of nickel(II) bromide at RT under N2. The concentration was halved by the introduction of additional NMP under -N2 and the solution was gently warmed to 200+ 5C and stirred for 4 days under N2. The reaction mixture was allowed to cool to room temperature. The reaction mixture was diluted with 30 volumes of tert-butyl methyl ether (MTBE) and filtered through celite. The celite pad was then rinsed with 10 volumes of MTBE. The organics were washed with 40 volumes of brine, 2 x 40 volumes of water and 40 volumes of brine. The combined organics were dried over sodium sulfate and concentrated to afford a brown solid, which was dried under vacuum (-30 in Hg) at 400C for 8 hours to afford the compound of Formula 3B (71% 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, 3-Chloro-2-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CYTOKINETICS, INC.; WO2007/75377; (2007); A2;,
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 933190-51-3 as follows. name: 8-Bromo-6-chloroimidazo[1,2-b]pyridazine

A mixture of 8-bromo-6-chloroimidazo[1,2-b]pyridazine (573 mg, 2.47 mmol), 6-(3-tert-butylpyrrolidin-1-yl)pyridin-2-amine (540 mg, 2.47 mmol), Pd2(dba)3 (142 mg, 0.25 mmol), BINAP (307 mg, 0.50 mmol), Cs2CO3 (2.4 g, 7.41 mmol) and dioxane (20 mL) was heated to reflux with stirring for 15 h under N2. The solvent was removed in vacuo and the resulting mixture was purified by chromatography (silica gel, 200-300 mesh, dichloromethane_MeOH=50:1) to give N-(6-(3-tert-butylpyrrolidin-1-yl)pyridin-2-yl)-6-chloroimidazo[1,2-b]pyridazin-8-amine (400 mg, crude) as a brown oil. LC-MS: [M+H]+, 371.1, tR=2.23 min.

According to the analysis of related databases, 933190-51-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hoffmann-La Roche Inc.; Hermann, Johannes Cornelius; Kuglstatter, Andreas; Lucas, Matthew C.; Padilla, Fernando; Wanner, Jutta; Zhang, Xiaohu; US2013/109661; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics