HRID1762839

反应详情

EQUATION

反应方程式

HRID 1762839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the product of part (ii) above (17.0 g) and 5N aqueous hydrochloric acid (150 ml) was heated under reflux for 3 hours. The resulting solution was evaporated and the residue was dissolved in the minimum volume of water. The solution was made basic (to a pH of about 8-9) by the addition of solid sodium bicarbonate. The solid was filtered off, washed with a little water and crystallised from ethanol/methanol (2:1) to give the title compound, (7.70 g), m.p. 229°-230°.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. customThe resulting solution was evaporated
  4. dissolutionthe residue was dissolved in the minimum volume of water
  5. additionby the addition of solid sodium bicarbonate
  6. filtrationThe solid was filtered off
  7. washwashed with a little water
  8. customcrystallised from ethanol/methanol (2:1)