Hydrazine → HCID 178509275、化合物

HRID 636418ノート

反応式

HRID 636418 の反応式
[NH2:1]N.[C:3]1([S:9]([C:12](=[CH:15][N:16](C)C)[C:13]#[N:14])(=[O:11])=[O:10])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>CCO>[C:3]1([S:9]([C:12]2[C:15]([NH2:16])=[N:1][NH:14][CH:13]=2)(=[O:10])=[O:11])[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

参加物

4

反応物 2

HCID 9321HydrazineHCID 42101212-(Benzenesulfonyl)-3-(dimethylamino)prop-2-enenitrile

生成物 1

HCID 178509275HCID 178509275、化合物収率 30%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2.05 ml (40.9 mmol) of NH2NH2 were added to a solution of 9.08 g (38.3 mmol) of 2-benzenesulphonyl-3-dimethylamino-acrylonitrile in 60 ml of EtOH and stirred at 40° for 5 hrs. The reaction solution was evaporated and the residue was partitioned between H2O and CH2Cl2. The aqueous phase was washed three times with CH2Cl2, and the combined organic phases were dried (MgSO4), filtered and evaporated. Chromatography (SiO2, CH2Cl2/MeOH 10:1) yielded 2.5 g (30%) of 4-benzenesulphonyl-1H-pyrazol-3-ylamine as a beige powder, m.p. 159-161°.

後処理

  1. customThe reaction solution was evaporated
  2. customthe residue was partitioned between H2O and CH2Cl2
  3. washThe aqueous phase was washed three times with CH2Cl2
  4. dry with materialthe combined organic phases were dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-3b4f7ae3e20142189dc167d1f135ee98
出典データセット
uspto-grants-2001_02
特許番号
US06194410B1

反応ノート

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