HRID1684631

反应详情

EQUATION

反应方程式

HRID 1684631 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2.1 g (4.91 mmole) of the product from Example 125, 25 mL 48% hydrobromic acid and 25 mL glacial acetic acid was refluxed for 18 hours. The mixture was poured into a stirred slurry of ice and water and stirred for 1 hour. The mixture was filtered, and the filtrant washed with water and dried to give a solid. Flash chromatography on silica gel eluting with 5% methanol in dichloromethane afforded 1.89 g (93%) the title product as a solid, mp 232°-234° C.

WORKUP

后处理

  1. temperaturewas refluxed for 18 hours
  2. filtrationThe mixture was filtered
  3. washthe filtrant washed with water
  4. customdried
  5. customto give a solid