3-Hydroxy-1-methylpiperidin-2-one → 1-Methylpiperidine-2,3-dione
反応式
[OH:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]([CH3:8])[C:3]1=[O:9]>CC(C)=O>[CH3:8][N:4]1[CH2:5][CH2:6][CH2:7][C:2](=[O:1])[C:3]1=[O:9]参加物
3
実験手順
To a solution of 3-hydroxy-1-methylpiperidin-2-one (1 g, 7.59 mmol) in acetone (50 mL) was added Jones-reagent (2 mL) dropwise at room temperature. The resulting solution was stirred for 10 min at room temperature. The solid material was removed by filtration. The filtrate was concentrated in vacuo at 30-40° C. The residue was dissolved in DCM (50 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to afford the title compound (220 mg, 11%) which was used in next step immediately without further purification.
後処理
- customThe solid material was removed by filtration
- concentrationThe filtrate was concentrated in vacuo at 30-40° C
- dissolutionThe residue was dissolved in DCM (50 mL)
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-308f8ff7226d40c1855d94c7c009a4fb
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08901313B2
反応ノート
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