HRID1043529

反应详情

EQUATION

反应方程式

HRID 1043529 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionadded slowly
  2. customto quench
  3. customreaction
  4. custompartitioned
  5. washorganic phases were washed by saturated saline
  6. concentrationfollowed by sodium sulphate drying, concentration, column chromatography (PE: EA=20:1)
  7. customto give 0.6 g light yellow gel-like substance, yield: 34%