反応式
[C:1]1([N:7]([CH2:11][C:12]([O:14]CC)=[O:13])[CH2:8][CH2:9][CH3:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>C(O)C.[OH-].[Na+]>[C:1]1([N:7]([CH2:11][C:12]([OH:14])=[O:13])[CH2:8][CH2:9][CH3:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1参加物
4
実験手順
To a solution of the product obtained in EXAMPLE 108 (5.0 g) in ethanol (30 ml), 3N aqueous sodium hydroxide (30 ml) was added and the mixture was stirred for 10 minutes under reflux. The aqueous solution was concentrated under reduced pressure and washed with ether, acidified to pH 3 with 2N hydrochloric acid and extracted four times with ethyl acetate. The combined organic layer was washed with saturated sodium chloride, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was crystallized from ethyl acetate-hexane to give 2.96 g (68%) of the objective compound.
後処理
- temperatureunder reflux
- concentrationThe aqueous solution was concentrated under reduced pressure
- washwashed with ether
- extractionextracted four times with ethyl acetate
- washThe combined organic layer was washed with saturated sodium chloride
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was crystallized from ethyl acetate-hexane
出典と根拠
- ORDレコード
- ord-18dcf2fbcc354b17936cdd9df7f79616
- 出典データセット
- uspto-grants-1995_03
- 特許番号
- US05397781
関連ノート
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