HRID977905

反应详情

EQUATION

反应方程式

HRID 977905 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 115 gm of the acid of Step A in 3.5 1. of methanol and add slowly 25 cc of sulfuric acid. Stir under reflux for 72 hours. Cool the reaction mixture to room temperature.and add 100 gm of sodium bicarbonate in portions. Stir for an additional hour, filter and strip the filtrate to dryness. Dissolve the residue in methylene chloride and wash the solution three times with water. Dry the solution and strip to an oil which solidifies. (m.p. 82°-84° C.).

WORKUP

后处理

  1. temperatureunder reflux for 72 hours
  2. stirringStir for an additional hour
  3. filtrationfilter
  4. dissolutionDissolve the residue in methylene chloride
  5. washwash the solution three times with water
  6. customDry the solution and strip to an oil which