Ethanol → HCID 309391、化合物
反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]([CH3:17])=[CH:11][C:12]([O:14]CC)=[O:13])=[CH:6][CH:5]=1)([O-:3])=[O:2].C(O)C.[OH-].[K+].O>C(OCC)(=O)C>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([C:10]([CH3:17])=[CH:11][C:12]([OH:14])=[O:13])=[CH:8][CH:9]=1)([O-:3])=[O:2]参加物
6
実験手順
A mixture of 16.6 g. of ethyl 3-(4-nitrophenyl)-2-butenoate, 75 ml. of ethanol and 94.7 ml. of 1.5 N potassium hydroxide was heated on a steam bath for 70 minutes, and then it was cooled to room temperature. To the reaction mixture was added 200 ml. of water and 200 ml. of ethyl acetate. The aqueous phase was removed and acidified with concentrated hydrochloric acid, and then the solid was recovered by filtration. This latter solid was recrystallized from aqueous ethanol to give 9.8 g. (67% yield) of the title compound, m.p. 167°-169° C.
後処理
- additionA mixture of 16.6 g
- additionTo the reaction mixture was added 200 ml
- customThe aqueous phase was removed
- filtrationthe solid was recovered by filtration
- customThis latter solid was recrystallized from aqueous ethanol
- customto give 9.8 g
出典と根拠
- ORDレコード
- ord-d6d944dfea2245e5af1a612c24b763b8
- 出典データセット
- uspto-grants-1982_08
- 特許番号
- US04343813
反応ノート
読み込み中…