Trifluoroacetic acid → Ethyl 3-hydroxy-4-oxopiperidine-1-carboxylate
反応式
[OH:1][CH:2]1[C:7](OC)([O:8]C)[CH2:6][CH2:5][N:4]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:3]1.FC(F)(F)C(O)=O>C1COCC1>[OH:1][CH:2]1[C:7](=[O:8])[CH2:6][CH2:5][N:4]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:3]1参加物
4
実験手順
Ethyl 3-hydroxy-4,4-dimethoxypiperidine-1-carboxylate from Example 34A (5.00 g, 21.4 mmol) was dissolved in THF (50 mL), and trifluoroacetic acid (15.9 mL, 214 mmol) was added. The mixture was stirred for 3.5 h at rt. The solvent was then removed in vacuo. Twice, toluene was added and again removed in vacuo. The residue was dissolved in dichloromethane, dried over sodium sulfate, and the solvent was removed in vacuo to yield 4.70 g (95%) of an oil, which was used without further purification.
後処理
- customThe solvent was then removed in vacuo
- additionTwice, toluene was added
- customagain removed in vacuo
- dissolutionThe residue was dissolved in dichloromethane
- dry with materialdried over sodium sulfate
- customthe solvent was removed in vacuo
出典と根拠
- ORDレコード
- ord-0f23eb935e624549bb2a1931a2483b84
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524722B2
反応ノート
読み込み中…