Sulfuric Acid → 2,4,5-Trifluoro-3-methoxybenzamide
反応式
S(=O)(=O)(O)[OH:2].[CH3:6][O:7][C:8]1[C:9]([F:18])=[C:10]([CH:13]=[C:14]([F:17])[C:15]=1[F:16])[C:11]#[N:12]>O>[CH3:6][O:7][C:8]1[C:9]([F:18])=[C:10]([CH:13]=[C:14]([F:17])[C:15]=1[F:16])[C:11]([NH2:12])=[O:2]参加物
4
実験手順
5 ml of concentrated sulfuric acid and 1.2 ml of water were added to 1.24 g (0.007 mole) of 3-methoxy-2,4,5-trifluorobenzonitrile (XXIV) [prepared as described in Step (E4) above], and the mixture was heated at 100°-140° C. for 30 minutes, poured into ice-water, and extracted with ethyl acetate. The extract was washed with water and dried, and the solvent was removed by evaporation under reduced pressure to afford 1.10 g of 3-methoxy-2,4,5-trifluorobenzamide (XXV) as a pale brown powder melting at 131°-133° C.
後処理
- temperaturethe mixture was heated at 100°-140° C. for 30 minutes
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- customdried
- customthe solvent was removed by evaporation under reduced pressure
出典と根拠
- ORDレコード
- ord-90feeeeb002248bbac841809afc0ca20
- 出典データセット
- uspto-grants-1991_03
- 特許番号
- US04997943
反応ノート
読み込み中…