Methanol → (S)-Methyl piperidine-2-carboxylate
反応式
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][C@H:2]1[C:7]([OH:9])=[O:8].S(Cl)(Cl)=O.[CH3:14]O>>[CH3:14][O:8][C:7]([C@@H:2]1[CH2:3][CH2:4][CH2:5][CH2:6][NH:1]1)=[O:9]参加物
4
実験手順
To a mixture of (S)-piperidine-2-carboxylic acid (10 mmol, 1.29 g) in MeOH (20 mL) is dropwise added thionyl chloride (30 mmol, 2.17 mL) at room temperature. The mixture is stirred at 2 hours, and then concentrated under reduced pressure. To the residue is added water (5 mL) and basified with potassium carbonate. The mixture is extracted with CH2Cl2. The combined organic layer is dried over Na2SO4, filtrated, and concentrated under reduced pressure to give (S)-piperidine-2-carboxylic acid methyl ester as a pale brown oil (800 mg, 56%).
後処理
- customat room temperature
- concentrationconcentrated under reduced pressure
- additionTo the residue is added water (5 mL)
- extractionThe mixture is extracted with CH2Cl2
- dry with materialThe combined organic layer is dried over Na2SO4
- filtrationfiltrated
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-0cdca4ad2b6240f19189e7439f27417c
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08759365B2
反応ノート
読み込み中…