Hydrazine hydrate (1:1) → HCID 178434193、化合物

HRID 1700640ノート

反応式

HRID 1700640 の反応式
[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

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 178467259HCID 178467259、化合物

生成物 1

HCID 178434193HCID 178434193、化合物収率 87.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-df408351dde541fbad1a26fda9ba44ec
出典データセット
uspto-grants-2002_02
特許番号
US06350749B1

反応ノート

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