Hydrazine hydrate (1:1) → 3,5-Difluorophenylhydroxyacetohydrazide
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:9]([OH:14])[C:10](OC)=[O:11])[CH:5]=[C:6]([F:8])[CH:7]=1.O.[NH2:16][NH2:17]>CC(O)C>[F:1][C:2]1[CH:3]=[C:4]([CH:9]([OH:14])[C:10]([NH:16][NH2:17])=[O:11])[CH:5]=[C:6]([F:8])[CH:7]=1参加物
4
実験手順
5.0 g of methyl 3,5-difluorophenylhydroxyacetate (C2) are dissolved in 45.0 ml of 2-propanol. 1.32 ml of hydrazine hydrate are then added dropwise, and the reaction mixture is kept under reflux for 18 hours. The solution is subsequently evaporated to dryness, and the resultant residue is purified by flash chromatography on silica gel (gradient for elution: ethyl acetate/0-20.0% by vol. of methanol), giving 3.70 g of the title compound as colourless solid having a melting point of 119.3° C. (MS: 202.8 (MH+)).
後処理
- temperatureunder reflux for 18 hours
- customThe solution is subsequently evaporated to dryness
- customthe resultant residue is purified by flash chromatography on silica gel (gradient for elution: ethyl acetate/0-20.0% by vol. of methanol)
出典と根拠
- ORDレコード
- ord-6c9a7b06ef9a497d8312c309b2e18cad
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08546613B2
反応ノート
読み込み中…