HRID907465

反应详情

EQUATION

反应方程式

HRID 907465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture containing the ester 18 (21.11 g, 89.4 mmol) and 10 M NaOH (36 ml, 4 equiv) in THF (220 ml), MeOH (110 ml) and water (55 ml) was stirred at reflux for 4 days. Half-saturated NH4Cl (600 ml) and AcOH (25 ml) were then added and the acid 19 was extracted into i-PrOAc. The organics were dried over Na2SO4 and concentrated. Trituration of the residue in ether:hexane 1:3 (200 ml) yielded 18.15 g (91%) of 19 as a white solid.

WORKUP

后处理

  1. temperatureat reflux for 4 days
  2. extractionthe acid 19 was extracted into i-PrOAc
  3. dry with materialThe organics were dried over Na2SO4
  4. concentrationconcentrated