HRID1615415
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of tert-butyl (3R)-3-[4-(hydroxymethyl)phenyl]morpholine-4-carboxylate 10 (6 g, 20.45 mmol) in THF (121.4 mL) was added manganese dioxide (17.78 g, 204.5 mmol) and the resulting mixture stirred at rt overnight. The reaction mixture filtered through pad of celite, and washed with EtOAc (3×50 mL). The filtrate was concentrated in vacuo to leave product as a colourless oil (5.54 g, 93% yield), which was used directly in the next step without further purification; 1H NMR (400.0 MHz, DMSO) d 1.39 (9H, s), 3.05 (1H, m), 3.52 (1H, m), 3.71-3.87 (4H, m), 4.28 (1H, m), 5.06 (1H, s), 7.55 (2H, m), 7.93 (2H, m) and 10.00 (1H, s) ppm
WORKUP
后处理
- filtrationThe reaction mixture filtered through pad of celite
- washwashed with EtOAc (3×50 mL)
- concentrationThe filtrate was concentrated in vacuo