Water → HCID 178434678、化合物

HRID 17831ノート

反応式

HRID 17831 の反応式
O.[NH2:2][NH2:3].C(O[C:7](=[C:9]([C:12]#[N:13])[C:10]#[N:11])[CH3:8])C.O>CCO>[NH2:11][C:10]1[NH:3][N:2]=[C:7]([CH3:8])[C:9]=1[C:12]#[N:13]

参加物

5

反応物 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 79450(1-Ethoxyethylidene)malononitrile

生成物 1

HCID 178434678HCID 178434678、化合物収率 71.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
95 °C

実験手順

Hydrazine monohydrate (6.8 ml, 0.14 mol) was dissolved in EtOH (10 ml) and cooled to 0° C. (1-Ethoxyethylidene)malononitrile (10 g, 0.073 mol) was added slowly and the mixture was heated at 95° C. for 2 h. After cooling to rt, water (20 ml) was added and the mixture was allowed to stand at rt overnight. The mixture was concentrated under reduced pressure and the resulting residue treated with EtOH (6 ml) and water (6 ml). After cooling in an ice/water bath for 10 min, the resulting precipitate was collected by filtration to give 6.34 g of 5-amino-3-methyl-1H-pyrazole-4-carbonitrile.

後処理

  1. additionwas added slowly
  2. temperatureAfter cooling to rt
  3. concentrationThe mixture was concentrated under reduced pressure
  4. additionthe resulting residue treated with EtOH (6 ml) and water (6 ml)
  5. temperatureAfter cooling in an ice/water bath for 10 min
  6. filtrationthe resulting precipitate was collected by filtration

出典と根拠

ORDレコード
ord-d69380414ccc4fa79cd8e846802ba5e2
出典データセット
uspto-grants-2010_06
特許番号
US07741318B2

反応ノート

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