Dimethylamine → N,N,1,3-tetramethyl-4-nitropyrazole-5-carboxamide

HRID 2058609노트

반응식

HRID 2058609 반응식
[CH3:1][N:2]1[C:6]([C:7](Cl)=[O:8])=[C:5]([N+:10]([O-:12])=[O:11])[C:4]([CH3:13])=[N:3]1.[CH3:14][NH:15][CH3:16].C(=O)([O-])[O-].[K+].[K+]>C(Cl)Cl>[CH3:14][N:15]([CH3:16])[C:7]([C:6]1[N:2]([CH3:1])[N:3]=[C:4]([CH3:13])[C:5]=1[N+:10]([O-:12])=[O:11])=[O:8]

참가 물질

5

반응물 3

HCID 674DimethylamineHCID 11430Potassium CarbonateHCID 103756241,3-Dimethyl-4-nitro-5-pyrazolecarboxylic acid chloride

생성물 1

HCID 20549790N,N,1,3-tetramethyl-4-nitropyrazole-5-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 40 g of 1,3-dimethyl-4-nitropyrazole--5-carboxylic acid chloride in 50 ml of methylene chloride is added dropwise at from 10° to 20° C., while cooling, to 43 g of a 40% strength aqueous solution of dimethylamine; stirring is continued for a further 20 minutes. The resulting mixture is rendered alkaline with potassium carbonate; the organic layer is separated off, and the aqueous phase is extracted by shaking it with methylene chloride. The organic solution is dried and concentrated, and the residue is triturated with petroleum ether (bp 40° to 70° C.) to yield 38.3 g of N,N,1,3-tetramethyl-4-nitropyrazole-5-carboxamide, mp 57° to 59.5° C., which is converted into a product of mp 114° to 115.5° C. on recrystallization from cyclohexane.

후처리

  1. customthe organic layer is separated off
  2. extractionthe aqueous phase is extracted
  3. stirringby shaking it with methylene chloride
  4. customThe organic solution is dried
  5. concentrationconcentrated
  6. customthe residue is triturated with petroleum ether (bp 40° to 70° C.)

출처 및 근거

ORD 기록
ord-b4dc527967fb49e68bdb72c91070988d
출처 데이터셋
uspto-grants-1982_03
특허 번호
US04317823

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