Category: 15953-45-4

Synthetic Route of 15953-45-4, A common heterocyclic compound, 15953-45-4, name is 5-Chloro-3-methyl-1H-pyrazole, molecular formula is C4H5ClN2, 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 solution ofKMnC>4 (3.5 g, 22 mmol) in water (120 mL) was added in portions over aperiod of 5 h at 70 C to a solution of5-chloro-3-methylpyrazole (1.0 g, 8.8 mmol; see step (c) above) in water (50 mL) and fc/^-butanol (1 mL). The mixture was stirred at 70 C overnight and filtered through Celite. The colourless filtrate was concentrated and acidified with HC1 (2M). Filtration gave the title compound as a white powder which was used without further purification. (Yield: 913 mg, 80%). ^-NMR (DMSO-dg): 5 13.65 (br s, 1H), 6.80 (s, 1H), 4.40 (bs, 1H).; A mixture of5-chloro-3-methylpyrazole (3.6 mmol; see step (a) above), water (6 mL), /e/Y-butanol (1.2 mL) and KMn04 (1.42 g, 9 mmol) was stirred at 75 C overnight. The hot mixture was filtered and the solids washed with boiling water. The combined filtrates were extracted twice with EtOAc. The combined extracts were washed with Nad (aq, sat), dried (MgS04) and concentrated to provide a solid, which was crystallised from EtOAc/hexane/pentane to give the sub-title product as white crystals (Yield: 350 mg (67%)). ‘H-NMR (DMSO-dg, 400 MHz), 5 13.65 (br s, 1H), 6.80 (s, 1H), 4.40 (bs, 1H).

The synthetic route of 15953-45-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOLIPOX AB; WO2006/32851; (2006); A1;,
Pyrazole – Wikipedia,
Pyrazoles – 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. 15953-45-4, name is 5-Chloro-3-methyl-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 15953-45-4

(b) S-Chloropyrazole-S-carboxylic acidA mixture of 5-chloro-3-methylpyrazole (3.6 mmol; see step (a) above), water (6 mL) and fert-butanol (1.2 mL) was heated to 750C, after which KMnO4 (1.42 g, 9 mmol) was added. The mixture was stirred at 75 C overnight and filtered hot. The solids were washed with boiling water. The combined cooled filtrates were extracted with EtOAc, and the combined extracts washed with NaCl (sat., aq.), dried (MgSO4) and concentrated. The crude solid was recrystallised from EPO EtOAc/hexane/pentane to give the sub-title compound as white crystals (Yield:350 mg (67%)).1H-NMR (DMSO-d6, 400 MHz), delta 13.65 (br s, IH), 6.80 (s, IH)

According to the analysis of related databases, 15953-45-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BIOLIPOX AB; WO2007/45868; (2007); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Synthetic Route of 15953-45-4, These common heterocyclic compound, 15953-45-4, name is 5-Chloro-3-methyl-1H-pyrazole, 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) 5-Chloropyrazole-3-carboxylic acid..A mixture of 5-chloro-3-methylpyrazole (3.6 mmol; see step (a) above), water (6 mL) and terf-butanol (1.2 mL) was heated to 750C, after which KMnO4 (1.42 g, 9 mmol) was added. The mixture was stirred at 75C overnight and filtered hot. The solids were washed with boiling water. The combined cooled filtrates were extracted with EtOAc, and the combined extracts washed with NaCI (sat., aq.), dried (MgSO4) and concentrated. The crude solid was recrystallised from EtOAc/hexane/pentane to give the sub-title compound as white crystals (Yield: 350 mg (67%)). 1H-NMR (DMSO-d6, 400 MHz), delta 13.65 (br s, 1 H), 6.80 (s, 1 H). (d) 5-Chloropyrazole-3-carboxylic acid. A solution of KMnO4 (3.5 g, 22 mmol) in water (120 mL) was added in portions over a period of 5 h at 700C to a solution of 5-chloro-3-methylpyrazole (1.0 g, 8.8 mmol; see step (c) above) in water (50 mL) and terf-butanol (1 mL). The mixture was stirred at 7O0C overnight and filtered through Celite. The colourless filtrate was concentrated and acidified with HCI (aq., 2M). Filtration gave the title compound as a white powder which was used without further purification. (Yield: 913 mg, 80%). 1H-NMR (DMSO-d6): delta 6.80 (s, 1 H), 4.40 (br s, 1 H).

Statistics shows that 5-Chloro-3-methyl-1H-pyrazole is playing an increasingly important role. we look forward to future research findings about 15953-45-4.

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. 15953-45-4, name is 5-Chloro-3-methyl-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C4H5ClN2

(b) S-Chloropyrazole-S-carboxylic acidA mixture of 5-chloro-3-methylpyrazole (3.6 mmol; see step (a) above), water (6 mL) and fert-butanol (1.2 mL) was heated to 750C, after which KMnO4 (1.42 g, 9 mmol) was added. The mixture was stirred at 75 C overnight and filtered hot. The solids were washed with boiling water. The combined cooled filtrates were extracted with EtOAc, and the combined extracts washed with NaCl (sat., aq.), dried (MgSO4) and concentrated. The crude solid was recrystallised from EPO EtOAc/hexane/pentane to give the sub-title compound as white crystals (Yield:350 mg (67%)).1H-NMR (DMSO-d6, 400 MHz), delta 13.65 (br s, IH), 6.80 (s, IH)

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 15953-45-4.