Hydrazine hydrate (1:1) → HCID 178434193, 화합물

HRID 1700640노트

반응식

HRID 1700640 반응식
[Cl:1][C:2]1[S:3][C:4]([Cl:18])=[CH:5][C:6]=1[CH:7]1[CH2:12][C:11](=O)[C:10](=[C:14](O)[CH3:15])[C:9](=[O:17])[CH2:8]1.O.[NH2:20][NH2:21]>C(O)C>[Cl:1][C:2]1[S:3][C:4]([Cl:18])=[CH:5][C:6]=1[CH:7]1[CH2:12][C:11]2[NH:21][N:20]=[C:14]([CH3:15])[C:10]=2[C:9](=[O:17])[CH2:8]1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 178467259HCID 178467259, 화합물

생성물 1

HCID 178434193HCID 178434193, 화합물수율 87.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 5-(2,5-dichlorothiophen-3-yl)-2-(1-hydroxyethylidene)cyclohexane-1,3-dione (2.48 g) and hydrazine hydrate (0.508 g) in ethanol (10 ml) was refluxed for 2 hours. Under reduced pressure, the solvent was evaporated, and to the residue was added water. The mixture was extracted with ethyl acetate, and the organic layer was washed with water and concentrated under reduced pressure. The residue was washed with diisopropylether to give 6-(2,5-dichlorothiophen-3-yl)-3-methyl-4,5,6,7-tetrahydroindazol-4-one (2.15 g) as pale yellow crystals.

후처리

  1. customUnder reduced pressure, the solvent was evaporated
  2. additionto the residue was added water
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe organic layer was washed with water
  5. concentrationconcentrated under reduced pressure
  6. washThe residue was washed with diisopropylether

출처 및 근거

ORD 기록
ord-df408351dde541fbad1a26fda9ba44ec
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06350749B1

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