Ethanol → tert-Butyl 4-[4-(2-cyclohexyl-N-methoxyethanimidoyl)-1,3-thiazol-2-yl]piperidine-1-carboxylate
反応式
[Cl-].CO[NH3+].[CH3:5][O:6][N:7](C)[C:8]([C:10]1[N:11]=[C:12]([CH:15]2[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH2:16]2)[S:13][CH:14]=1)=O.O.[CH2:30](O)[CH3:31]>>[CH:30]1([CH2:31][C:8]([C:10]2[N:11]=[C:12]([CH:15]3[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH2:16]3)[S:13][CH:14]=2)=[N:7][O:6][CH3:5])[CH2:19][CH2:20][CH2:15][CH2:16][CH2:17]1参加物
5
反応条件
- 温度
- 50 °C
実験手順
At room temperature, methoxyammonium chloride (171 mg) was added to a solution of tert-butyl 4-{4-[methoxy(methyl)carbamoyl]-1,3-thiazol-2-yl}piperidine-1-carboxylate (403 mg) in ethanol (2 ml). The reaction mixture was stirred at 50° C. for 24 hours, and water was then added. The aqueous phase was separated off and extracted with ethyl acetate. The combined organic phases were dried over sodium sulphate and concentrated under reduced pressure. The residue was purified chromatographically. This gave tert-butyl 4-[4-(2-cyclohexyl-N-methoxyethanimidoyl)-1,3-thiazol-2-yl]piperidine-1-carboxylate (361 mg).
後処理
- customThe aqueous phase was separated off
- extractionextracted with ethyl acetate
- dry with materialThe combined organic phases were dried over sodium sulphate
- concentrationconcentrated under reduced pressure
- customThe residue was purified chromatographically
出典と根拠
- ORDレコード
- ord-3ae44a1cde364a1eae928f090857ef4c
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09357779B2
反応ノート
読み込み中…