HRID487328

反应详情

EQUATION

反应方程式

HRID 487328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.0 g of 6-(2-(4-chlorobenzenesulphonylamino)indan-5-yl)-6-(3-pyridyl)hex-5-enoic acid are dissolved in 50 ml of 0.3N sodium hydroxide solution and hydrogenated with 1 g of palladium/charcoal at 40° C. and 3.5 bar for 12 hours. The catalyst is then removed by suction filtering and the filtrate is adjusted to pH 4 to 5. The product precipitated is separated off and taken up in chloroform. The organic extract is washed with water, dried and evaporated down. Then the mixture is chromatographed over a silica gel column using the eluant ethylene chloride/ethyl acetate/glacial acetic acid (70:30:2). The third fraction contains the desired product.

WORKUP

后处理

  1. customThe catalyst is then removed by suction
  2. filtrationfiltering
  3. customThe product precipitated
  4. customis separated off
  5. extractionThe organic extract
  6. washis washed with water
  7. customdried
  8. customevaporated down
  9. customThen the mixture is chromatographed over a silica gel column