HRID616261

反应详情

EQUATION

反应方程式

HRID 616261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 82.2 g (0.20 mol) of the compound of Example 10 in 300 ml of tetrahydrofuran and 700 ml of methanol was hydrogenated in the presence of 4 g of 5% sulfided platinum on carbon at room temperature and 1500 psi for 22 hours. The reaction mixture was concentrated and the solid residue (76 g) was recrystallized from ethanol (320 ml) to afford 61.4 g (81%) of light orange crystals, m.p. 151.5°-153°. The analytical sample was prepared by a second recrystallization from ethanol: white crystals, m.p. 152°-153.5°.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. customthe solid residue (76 g) was recrystallized from ethanol (320 ml)
  3. customto afford 61.4 g (81%) of light orange crystals, m.p. 151.5°-153°