HRID542133

反应详情

EQUATION

反应方程式

HRID 542133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 13 g (0.041 mol) of product of Example 35, 10 g of KOH, 100 ml of methanol, 100 ml of water was held at reflux for 20 hours, cooled, and poured into ice water (500 ml) containing 20 ml of concentrated HCl. The mixture was extracted with ether. The ether solution was dried and concentrated to give a solid which was recrystallized from hexane to give 4.68 g (39%) of product; mp 161°-162° C. A second crop, 4.74 g (40%), mp 155°-159° C., was obtained from mother liquor. Total yield was 79%.

WORKUP

后处理

  1. temperatureat reflux for 20 hours
  2. temperaturecooled
  3. extractionThe mixture was extracted with ether
  4. dry with materialThe ether solution was dried
  5. concentrationconcentrated
  6. customto give a solid which
  7. customwas recrystallized from hexane