HRID2952

反应详情

EQUATION

反应方程式

HRID 2952 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 0.28 g of the compound of Example 61 in 30 ml of tetrahydrofuran was hydrogenated at 60 pounds per square inch in the presence of 1.12 g of 5% palladium on carbon overnight at 60° C. The reaction mixture was filtered and evaporated to dryness. The resulting residue was dissolved in 3.5 ml of a 1:1.5 ethyl acetate/hexane solution and loaded onto a silica gel chromatography column. Elution with 40% ethyl acetate in hexane produced fractions which, upon evaporation to dryness, provided 0.05 g of title compound. m.p. 64°-68° C.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. customevaporated to dryness
  3. dissolutionThe resulting residue was dissolved in 3.5 ml of a 1:1.5 ethyl acetate/hexane solution
  4. washElution with 40% ethyl acetate in hexane produced fractions which
  5. customupon evaporation to dryness