反応式
[OH:1][C:2]1[CH:19]=[CH:18][C:5]2[S:6][C:7]3[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([OH:17])=[O:16])[C:8]=3[CH2:9][CH2:10][C:4]=2[CH:3]=1.Cl.[CH2:21](O)[CH3:22]>C(OCC)(=O)C.C1C=CC=CC=1>[OH:1][C:2]1[CH:19]=[CH:18][C:5]2[S:6][C:7]3[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([O:17][CH2:21][CH3:22])=[O:16])[C:8]=3[CH2:9][CH2:10][C:4]=2[CH:3]=1参加物
5
実験手順
An amount of 1.7 g of 2-hydroxy-9-carboxy-10,11-dihydrodibenzo[ b,f] thiepin was dissolved in 50 ml of anhydrous ethanol and the mixture was refluxed for 3 hours, while hydrogen chloride gas was bubbled into the mixture. The solvent was distilled off to obtain the residue which was dissolved in the mixed solvent of ethyl acetate-benzene. The solution was washed with saturated sodium chloride solution and freed of solvent by distillation to obtain 1.6 g (85%) of 2-hydroxy-9-ethoxycarbonyl-10,11-dihydrodibenzo[b,f]thiepin as brown crystals having a melting point of 125°-129° C.
後処理
- customwas bubbled into the mixture
- distillationThe solvent was distilled off
- customto obtain the residue which
- washThe solution was washed with saturated sodium chloride solution
- distillationfreed of solvent by distillation
出典と根拠
- ORDレコード
- ord-c5c03ba49e764c6689d82ebf3ba22f88
- 出典データセット
- uspto-grants-1979_08
- 特許番号
- US04166127
関連ノート
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