HRID1623666

反应详情

EQUATION

反应方程式

HRID 1623666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

LiOH (1.25 mL, 3.74 mmol) was added to a stirred solution of phenylmethyl 2-[(phenylmethyl)oxy]-5-(1-piperidinyl)benzoate (may be prepared as described in Description 41; 150 mg, 0.37 mmol) in a mixture of THF:water (3:1, 10 ml). The mixture was heated to reflux for 12 h and then diluted with ethyl acetate (50 ml). 10% aqueous HCl was added to the mixture to adjust the pH to 2. The organic phase was isolated, washed with brine, dried over magnesium sulphate, and concentrated to give a yellow oil. The crude product was purified using Comflash to yield the title compound. 80 mg.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 12 h
  3. customThe organic phase was isolated
  4. washwashed with brine
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated
  7. customto give a yellow oil
  8. customThe crude product was purified