tert-Butyl 4-formylpiperidine-1-carboxylate → tert-Butyl 4-(1-hydroxyethyl)piperidine-1-carboxylate
反応式
[CH:1]([CH:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][CH2:4]1)=[O:2].[CH3:16][Mg]Br>C1COCC1>[OH:2][CH:1]([CH:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][CH2:4]1)[CH3:16]参加物
4
反応条件
- 温度
- -78 °C
実験手順
Placed tert-butyl 4-formylpiperidine-1-carboxylate (2.00 g, 9.38 mmol) in THF (40 mL) and cooled to −78° C. Slowly added methylmagnesium bromide (3.44 mL, 10.3 mmol) stirred for 1 hour. Slowly added saturated ammonium chloride and extracted with CH2Cl2. Concentrated and redissolved in 5% MeOH in CH2Cl2. Added ether and filtered off solids. Concentrate filtrate to give the title compound (1.94 g, 90.2% yield)
後処理
- extractionSlowly added saturated ammonium chloride and extracted with CH2Cl2
- concentrationConcentrated
- dissolutionredissolved in 5% MeOH in CH2Cl2
- filtrationAdded ether and filtered off solids
出典と根拠
- ORDレコード
- ord-e866eee4ded14399b36a69408e9cf124
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08022223B2
反応ノート
読み込み中…