反応式
C([O:3][C:4]([CH:6]([C:14]1[CH:27]=[CH:26][C:25]2[S:24](=[O:29])(=[O:28])[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[N:17](C(OC(C)(C)C)=O)[C:16]=2[CH:15]=1)[CH2:7][CH:8]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1)=[O:5])C.[OH-].[Na+]>CO>[O:29]=[S:24]1(=[O:28])[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[NH:17][C:16]2[CH:15]=[C:14]([CH:6]([CH2:7][CH:8]3[CH2:13][CH2:12][O:11][CH2:10][CH2:9]3)[C:4]([OH:5])=[O:3])[CH:27]=[CH:26][C:25]1=2参加物
4
反応条件
- 温度
- 60 °C
実験手順
700 mg of tert-butyl 2-[1-ethoxycarbonyl-2-(tetrahydropyran-4-yl)ethyl]-5,5-dioxo-5H-phenothiazine-10-carboxylate are suspended in 50 ml of methanol, and 10 ml of 2 M NaOH solution are added. The reaction mixture is stirred at 60° C. for one hour. The methanol is removed under reduced pressure and the reaction mixture is adjusted to pH 4 by addition of concentrated hydrochloric acid. The mixture is extracted three times with in each case 100 ml of ethyl acetate. The combined organic phases are dried over MgSO4 and then concentrated under reduced pressure. This gives 600 mg of 2-(5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-3-(tetrahydropyran-4-yl)propionic acid. C20H21NO5S (387.46), LCMS (ESI): 388.1 (M+H+).
後処理
- customThe methanol is removed under reduced pressure
- additionthe reaction mixture is adjusted to pH 4 by addition of concentrated hydrochloric acid
- extractionThe mixture is extracted three times with in each case 100 ml of ethyl acetate
- dry with materialThe combined organic phases are dried over MgSO4
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-6181f8ec7ed14919a6aa6148667d3628
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732440B2
関連ノート
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