Sulfuric Acid → 4-Amino-1-methyl-5-methylaminopyrazole

HRID 1376889노트

반응식

HRID 1376889 반응식
Br[C:2]1[C:6]([N+:7]([O-])=O)=[C:5]([NH:10][CH3:11])[N:4]([CH3:12])[N:3]=1.S(=O)(=O)(O)O>O>[NH2:7][C:6]1[CH:2]=[N:3][N:4]([CH3:12])[C:5]=1[NH:10][CH3:11]

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 229186403-Bromo-1-methyl-5-methylamino-4-nitropyrazole

생성물 1

HCID 186927564-Amino-1-methyl-5-methylaminopyrazole수율 137.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

0.5 g (2.13 mmoles) of 3-bromo-1-methyl-5-methylamino-4-nitropyrazole are hydrogenated in a solution of 220 mg (2.13 mmoles) sulfuric acid in 20 ml water for 14 hours after adding the catalyst as described in method (2). After filtering the catalyst, the filtrate is reduced until dry and the residue is recrystallized from ethanol. 370 mg (78 percent of theory) of 4-amino-1-methyl-5-methylaminopyrazole hydrosulfate are obtained in the form of colorless crystals with a melting point of 185° to 188° C.

후처리

  1. additionafter adding the catalyst
  2. filtrationAfter filtering the catalyst
  3. customuntil dry
  4. customthe residue is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-4887a720c9b04feb9bb6099fe2063b4b
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05663366

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