HRID11218

反应详情

EQUATION

反应方程式

HRID 11218 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

The mixture of Isomer A of 4-((3,5-bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepan-2-one (90 mg, 0.20 mmol) in borone.THF complex solution (1.5 M in diethyl ether, 1.08 mL) was stirred at room temperature overnight and then at 65° C. for 1 hr. After cooling down, the mixture was concentrated under vacuum and methanol (0.4 mL) and 1N HCl solution (0.4 mL) was added and the mixture was stirred at 65° C. for 2 hr. After cooling down, the mixture was concentrated under vacuum and neutralized with 1N NaOH solution and extracted with dichloromethane 3 times. The combined organic layers were dried over magnesium sulfate, filtered and concentrated under vacuum to give the product as a clear colorless sticky oil (quantitative yield).

WORKUP

后处理

  1. temperatureAfter cooling down
  2. concentrationthe mixture was concentrated under vacuum and methanol (0.4 mL) and 1N HCl solution (0.4 mL)
  3. additionwas added
  4. temperatureAfter cooling down
  5. concentrationthe mixture was concentrated under vacuum
  6. extractionextracted with dichloromethane 3 times
  7. dry with materialThe combined organic layers were dried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum