Ethanol → 6,11-Dihydro-11-oxodibenz[b,e]oxepin-2-carboxylic acid ethyl ester
反応式
[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17](Cl)=[O:18])=[CH:16][C:3]1=2.[CH2:20]([OH:22])[CH3:21]>>[CH2:20]([O:22][C:17]([C:15]1[CH:14]=[CH:13][C:4]2[O:5][CH2:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[C:2](=[O:1])[C:3]=2[CH:16]=1)=[O:18])[CH3:21]参加物
実験手順
Next, 30.44 g of oxepincarboxylic acid III obtained above was allowed to react with 30 ml of thionyl chloride in 200 ml of toluene by heating under reflux for one hour. Concentration of the reaction mixture to dryness under reduced pressure gave 6,11-dihydro-11-oxodibenz[b,e]oxepin-2-carboxylic acid chloride IV in a quantitative yield. One half of this acid chloride IV was added to 300 ml of ethanol, and the mixture was stirred at room temperature for three hours and concentrated under reduced pressure. The residue was dissolved in chloroform, and the solution was washed with a saturated aqueous solution of sodium bicarbonate, dehydrated and concentrated to dryness to obtain 6,11-dihydro-11-oxodibenz[b,e]oxepin-2-carboxylic acid ethyl ester V in a quantitative yield. Recrystallization from n-hexane gave pure crystals having a melting point of 104°-105° C. IR spectrum (KBr tablet, cm-1): 2980, 1710, 1650, 1610, 1250, 1010.
後処理
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in chloroform
- washthe solution was washed with a saturated aqueous solution of sodium bicarbonate
- concentrationconcentrated to dryness
出典と根拠
- ORDレコード
- ord-9d0ce38ce1be440b934972a3162e1abf
- 出典データセット
- uspto-grants-1986_06
- 特許番号
- US04596804
反応ノート
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