HRID1043529
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- -20 °C
PROCEDURE
实验过程
4-hydroxy-4-(4-(trifluoromethoxy)phenyl)piperidine-1-formic acid tert-butyl ester (1.85 g, 5 mmol) was dissolved in dry dichloromethane (30 mL), cooled to −20° C., added dropwise triethyl silicane (696 mg, 6 mmol), added slowly until completed, slowly resumed to stir for 15 h at room temperature. After the reaction was finished, added ice water to quench reaction, partitioned, organic phases were washed by saturated saline, followed by sodium sulphate drying, concentration, column chromatography (PE: EA=20:1) to give 0.6 g light yellow gel-like substance, yield: 34%.
WORKUP
后处理
- additionadded slowly
- customto quench
- customreaction
- custompartitioned
- washorganic phases were washed by saturated saline
- concentrationfollowed by sodium sulphate drying, concentration, column chromatography (PE: EA=20:1)
- customto give 0.6 g light yellow gel-like substance, yield: 34%