Dichloromethane → HCID 21332190, compound

HRID 1390948Notes

Reaction equation

HRID 1390948 reaction equation
[C:1]([Cl:9])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.C(Cl)Cl.[CH3:13][N:14]1[C:18]2[C:19]3[CH:25]=[CH:24][CH:23]=[CH:22][C:20]=3[S:21][C:17]=2[C:16]([NH2:26])=[N:15]1>N1C=CC=CC=1>[ClH:9].[CH3:13][N:14]1[C:18]2[C:19]3[CH:25]=[CH:24][CH:23]=[CH:22][C:20]=3[S:21][C:17]=2[C:16]([NH:26][C:1]([C:2]2[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=2)=[O:8])=[N:15]1

Participants

5

Reactant 3

HCID 6344Dichloromethane2×HCID 82604Nicotinoyl chlorideHCID 70525418HCID 70525418, compound

Product 1

HCID 21332190HCID 21332190, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

A solution of 14.2 g. of nicotinic acid chloride in 100 ml. of methylene chloride was added to a stirred solution of 0.1 mole of 1-methyl-1H-(1)benzothieno-[3,2-c]pyrazol-3-amine in 400 ml. of methylene chloride containing 10 ml. of pyridine. The reaction mixture was stirred overnight at room temperature and the precipitate which formed was collected by filtration. Recrystallization from glacial acetic acid/concentrated hydrochloric acid gave N-(1-methyl-1H-(1)benzothieno[3,2-c]pyrazol-3-yl)-3-pyridinecarboxamide hydrochloride, m.p. 298°-300° C.

Workup

  1. customthe precipitate which formed
  2. filtrationwas collected by filtration
  3. customRecrystallization from glacial acetic acid/concentrated hydrochloric acid

Sources & evidence

ORD record
ord-0fc5736bc26a4266acf3e0134c5b6b80
Source dataset
uspto-grants-1979_02
Patent number
US04140785

Reaction notes

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