HRID1285257

反应详情

EQUATION

反应方程式

HRID 1285257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.2 g (2.2 mmole) of the compound of Example 28 dissolved in 20 ml ethanol and 35 ml tetrahydrofuran was saponified with 0.3 g NaOH, the reaction mixture acidified with dilute HCl to pH 3 and extracted with ethyl acetate. The organic phase was washed with water until neutral, then with brine and dried with magnesium sulfate. The crude residue after evaporation of the solvent was triturated with benzene and 0.18 (16%) of the title compound as a white solid, mp 95.5°-97.5° C., separated by filtration. Calc: C, 67.68; H, 7.44; Found: C, 67.56; H, 7.34.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic phase was washed with water until neutral, then with brine
  3. dry with materialdried with magnesium sulfate
  4. customThe crude residue after evaporation of the solvent
  5. customwas triturated with benzene and 0.18 (16%) of the title compound as a white solid, mp 95.5°-97.5° C.
  6. customseparated by filtration