HRID2198993

反应详情

EQUATION

反应方程式

HRID 2198993 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.9 cc of toluene containing 2.62 g (0.013 mole) of (CH3OCH2CH2O)2NaAlH2 is added to a solution of 4.13 g (0.0089 mole) of the compound of Example 16 in 80 cc of toluene and the obtained mixture is refluxed with stirring under argon atmosphere. After 6 hours, when the reaction, which is followed by thin layer chromatography, is completed, 100 cc of 5% NaOH is added to the mixture and the toluene phase is separated and washed with a saturated NaCl solution. Upon evaporating the solvent, a crude product is obtained which is recrystallized from ethyl acetate:hexane 1:1, yielding 2 g of the compound of the title. M.p. 144°-46° C.

WORKUP

后处理

  1. temperaturethe obtained mixture is refluxed
  2. customwhen the reaction, which
  3. customthe toluene phase is separated
  4. washwashed with a saturated NaCl solution
  5. customUpon evaporating the solvent
  6. customa crude product is obtained which
  7. customis recrystallized from ethyl acetate:hexane 1:1