Category: 1369959-12-5

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. 1369959-12-5, name is 3-Chloro-5-nitro-1H-pyrazole, A new synthetic method of this compound is introduced below., Computed Properties of C3H2ClN3O2

Tin (II) chloride (12.8 g, 68 mmol) was added in portions to a solution of 3-chloro-5-nitro- lH-pyrazole (2.0 g, 13.6 mmol) in methanol (200 mL) and cone. HCl (10 mL) at 0 C. The reaction mixture was stirred at room temperature for 6 hours, and the organic solvent was removed under reduced pressure. The residue was diluted with water (20 mL), neutralized to pH 7 with Na2C03, then extracted with EtOAc (3 x 50 mL). The combined organic phases were washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated to give the title compound (1.4 g, 87%), which was used without further purification. 1H NMR (400 MHz, DMSO-d6): delta 11.55 (bs, 1H), 5.26 (s, 2H), 5.21 (s, 1H).

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; CORNELL UNIVERSITY; DANA-FARBER CANCER INSTITUTE, INC.; CHILDREN’S MEDICAL CENTER CORPORATION; MELNICK, Ari, M.; GABAS, Lorena, Fontan; US, Ilkay; CASALENA, Gabriella; GRAY, Nathanael, S.; SCOTT, David, A.; HATCHER, John; DU, Guangyan; WU, Hao; QIAO, Qi; (157 pag.)WO2018/85247; (2018); A1;,
Pyrazole – Wikipedia,
Pyrazoles – 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. 1369959-12-5, name is 3-Chloro-5-nitro-1H-pyrazole, A new synthetic method of this compound is introduced below., name: 3-Chloro-5-nitro-1H-pyrazole

Aqueous HCI (16.8 mL, 544 mmol) was added over a period of 10 min to a solution of compound 1-1 b (4.0 g, 27.1 mmol) in MeOH (200 mL). The reaction mixture was cooled to 0 C and tin(ll) chloride (30.0 g, 158 mmol) was added portion wise and the resulting reaction mixture was stirred at rt. The progress of the reaction was monitored by TLC and after 16 h, when starting material was deemed consumed, the solvent was evaporated. The residue was diluted with EtOAc (100 mL) and 30% aqueous NaOH solution (120 mL) was added dropwise at 0 C until basic pH, then stirred at 0 C for 2h. Solid precipitates were filtered off through a pad of Celite and the cake was rinsed with EtOAc (50 mL) and water (50 mL). The organic phase was separated and the aqueous phase was extracted with EtOAc (50 mL). The combined organic layers were washed with brine (50 mL), dried (Na2S04), filtered and concentrated under vacuum which gave the title compound (3.5 g, 93 %). The compound was used in next step without further purification. MS (ES+) 1 18.04 [M+H]+.

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.

Electric Literature of 1369959-12-5, 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. 1369959-12-5, name is 3-Chloro-5-nitro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a solution of 3-methyl-5-nitro-lH-pyrazole (2.46 g, 19.40 mmol) and l -methyl-4- piperidinemethanol (5.00 g, 38.70 mmol) in dry Me-THF (190 mL). Di-tert-butyl azodicarboxylate (8.91 g, 38.70 mmol) and PPh3 (10.20 g, 38.70 mmol) were added. The solution was heated at 55 C over the weekend. The reaction mixture was diluted with EtOAc and water. The organic layer was separated and the aqueous layer was extracted thrice with EtOAc. The organic layers were combined, washed with brine, dried over MgS04, filtered and concentrated. The residue (yellow oil) was purified by column chromatography on silica gel (Irregular SiOH, 15-40 muiotaeta, 330 g, liquid loading in DCM, mobile phase: DCM/MeOH, gradient from 100:0 to 90: 10). The fractions containing the product were combined and evaporated to dryness to give 2.36 g of intermediate 195 (51% yield, yellow oil).

The chemical industry reduces the impact on the environment during synthesis 3-Chloro-5-nitro-1H-pyrazole. I believe this compound will play a more active role in future production and life.