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

HRID 1376889ノート

反応式

HRID 1376889 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 186927564-Amino-1-methyl-5-methylaminopyrazole収率 137.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-4887a720c9b04feb9bb6099fe2063b4b
出典データセット
uspto-grants-1997_09
特許番号
US05663366

反応ノート

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