反応式
[CH3:1][CH2:2][CH2:3][C:4]1[C:9]([OH:10])=[C:8]([C:11]([CH3:13])=[O:12])[CH:7]=[CH:6][C:5]=1[OH:14].[C:15]([O:22]C)(=[O:21])[CH2:16][CH2:17][C:18]([CH3:20])=O.N1CCCC1>C1(C)C=CC=CC=1>[OH:14][C:5]1[CH:6]=[CH:7][C:8]2[C:11](=[O:12])[CH2:13][C:18]([CH2:17][CH2:16][C:15]([OH:22])=[O:21])([CH3:20])[O:10][C:9]=2[C:4]=1[CH2:3][CH2:2][CH3:1]参加物
5
実験手順
To a mixture of 20.0 g (103 mmole) of 2,4-dihydroxy-3-propylacetophenone and 15.5 g (134 mmole) of methyl levulinate in 100 ml of dry toluene was added by syringe 21.5 ml (ca. 260 mmole) of pyrrolidine. After stirring for one hour the solution was heated on a steam bath for four hours and allowed to cool. The toluene solution was washed with water and 2N NaOH. The basic solution was acidified and extracted with diethyl ether, which in turn was extracted with saturated sodium bicarbonate. The basic aqueous extract was neutralized with dilute hydrochloric acid and again extracted with diethyl ether. After drying, the solution was concentrated at reduced pressure to an oil which crystallized to the title compound, m.p. 152°-153°.
後処理
- temperaturewas heated on a steam bath for four hours
- temperatureto cool
- washThe toluene solution was washed with water and 2N NaOH
- extractionextracted with diethyl ether, which in turn
- extractionwas extracted with saturated sodium bicarbonate
- extractionThe basic aqueous extract
- extractionagain extracted with diethyl ether
- customAfter drying
- concentrationthe solution was concentrated at reduced pressure to an oil which
- customcrystallized to the title compound, m.p. 152°-153°
出典と根拠
- ORDレコード
- ord-1d664d7a2fbd4c19bec6162263fba5f7
- 出典データセット
- uspto-grants-1988_10
- 特許番号
- US04778903
関連ノート
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