反応式
Cl.[Cl:2][C:3]1[C:13]2[CH2:12][CH2:11][NH:10][CH2:9][CH:8]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:7]=2[CH:6]=[C:5]([OH:20])[C:4]=1[OH:21].[F:22][C:23]([F:34])([F:33])[C:24]1[CH:32]=[CH:31][C:27]([C:28](Cl)=[O:29])=[CH:26][CH:25]=1.C(=O)(O)[O-].[Na+]>CC(C)=O.O>[Cl:2][C:3]1[C:13]2[CH2:12][CH2:11][N:10]([C:28](=[O:29])[C:27]3[CH:31]=[CH:32][C:24]([C:23]([F:22])([F:33])[F:34])=[CH:25][CH:26]=3)[CH2:9][CH:8]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:7]=2[CH:6]=[C:5]([OH:20])[C:4]=1[OH:21]参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
A solution of 0.74 g (0.002 mole) of 6-chloro-7,8-dihydroxy-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride, 0.55 g (0.0025 mole) of p-trifluoromethyl benzoylchloride, 0.17 g (0.002 mole) of sodium bicarbonate and 40 ml of 1:1 acetone-water solution was stirred overnight under nitrogen. The mixture was evaporated to dryness. The residue was extracted with ethylacetate. The extracted material was purified over a silica gel column using methanol-ethyl acetate to give 6-chloro-7,8-dihydroxy-1-phenyl-3-(p-trifluoromethylbenzoyl)-2,3,4,5-tetrahydro-1H-3-benzazepine, m.p. 243°-245° (dec.).
後処理
- customThe mixture was evaporated to dryness
- extractionThe residue was extracted with ethylacetate
- customThe extracted material was purified over a silica gel column
出典と根拠
- ORDレコード
- ord-3a7aa37e47b9480f8eaa7b9ac3db39d7
- 出典データセット
- uspto-grants-1981_03
- 特許番号
- US04255422
関連ノート
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