HRID28219

反应详情

EQUATION

反应方程式

HRID 28219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-{3-[3-[3-(1-Hydroxycyclohexyl)-2-propynyl]-4-oxo-2-thiazolidinyl]propyl}benzoic Acid (4.0 g., 0.01 mole) is dissolved in ethyl acetate (45 ml.) and hydrogenated at 25° C. and one atmosphere pressure over 1.0 g. of a 5% palladium on charcoal catalyst. When 0.01 mole of hydrogen is absorbed (2 hours), uptake of hydrogen becomes very slow. An additional 1.5 g. of catalyst is added and hydrogenation continued for 70 hours until 0.02 mole of hydrogen has been absorbed. The catalyst is removed by filtration and the solvent evaporated. The residual oil is chromatographed on silica gel with elution by 2% methanol in chloroform. The chromatographed product crystalizes when triturated with ether. There is obtained 1.2 g. of the title product, m.p. 118°-121° C.

WORKUP

后处理

  1. additionof catalyst is added
  2. customhas been absorbed
  3. customThe catalyst is removed by filtration
  4. customthe solvent evaporated
  5. customThe residual oil is chromatographed on silica gel with elution by 2% methanol in chloroform
  6. customThe chromatographed product crystalizes when
  7. customtriturated with ether
  8. customThere is obtained 1.2 g