HRID1462895

反应详情

EQUATION

反应方程式

HRID 1462895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 8.32 g (0.0185 mole) of the compound of Example 16, 0.9 g of 10% Pd-C catalyst, and 150 cc of tetrahydrofuran containing 20 cc of 1M NaOH is shaken in a Paar hydrogenator under about 5.4 atm. of hydrogen pressure until hydrogenolysis is completed. The catalyst is filtered and the mother liquor is concentrated to remove the solvent. The residue is taken up with methylene chloride, and washed with water. Upon evaporating the solvent, 6.1 g of a crude product are obtained which is recrystallized from acetone yielding 4.74 g of the compound of the title. M.p. 181.5°-182.5° C.

WORKUP

后处理

  1. filtrationThe catalyst is filtered
  2. concentrationthe mother liquor is concentrated
  3. customto remove the solvent
  4. washwashed with water
  5. customUpon evaporating the solvent, 6.1 g of a crude product
  6. customare obtained which
  7. customis recrystallized from acetone yielding 4.74 g of the compound of the title