Ammonia → 2,2-Difluoro-2-phenylacetamide
反応式
[F:1][C:2]([F:14])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:3](OCC)=[O:4].[NH3:15]>CCO>[F:1][C:2]([F:14])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:3]([NH2:15])=[O:4]参加物
4
実験手順
A solution of the title compound of Step (A) (6.00 g; 30 mmol) in 50 ml of EtOH was saturated with anhydrous NH3. An exothermic reaction was observed. After stirring the reaction mixture 60 hr at room temperature, the volatiles were removed in vacuo and the solid residue was taken up in a minimal amount of hot ethyl acetate. A small amount of insoluble material was filtered off and hexane was added to the filtrate until slightly turbid. After cooling to room temperature and standing several hr, the crystals were filtered and dried to afford 4.68 g (91%) of the title compound of this step as a colorless crystalline solid.
後処理
- customAn exothermic reaction
- customthe volatiles were removed in vacuo
- filtrationA small amount of insoluble material was filtered off
- additionhexane was added to the filtrate until slightly turbid
- temperatureAfter cooling to room temperature
- waitstanding several hr
- filtrationthe crystals were filtered
- customdried
出典と根拠
- ORDレコード
- ord-f969fd42a4e149a1a52bb36191ea5073
- 出典データセット
- uspto-grants-1998_12
- 特許番号
- US05846990
反応ノート
読み込み中…