Water → HCID 178434678, 화합물

HRID 17831

반응식

HRID 17831 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 178434678HCID 178434678, 화합물수율 71.1%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
95 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d69380414ccc4fa79cd8e846802ba5e2
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741318B2

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