HRID1244644

反应详情

EQUATION

反应方程式

HRID 1244644 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

30 g (70.7 mmol) of tert-butyl [4′-(2,4-dioxothiazolidin-5-ylidenemethyl)biphenyl-3-ylmethyl]methylcarbamate in 500 ml of dioxane are introduced into a three-necked flask. The reaction medium is degassed, 30 g of palladium on carbon (10%) are added and the mixture is hydrogenated at a pressure of 3 bar at 60° C. The reaction medium is filtered, evaporated off and the residue obtained is purified by chromatography on a silica column eluted with a dichloromethane and methanol (99–1) mixture. 18 g (60%) of the expected product are recovered after evaporation of the solvents.

WORKUP

后处理

  1. customThe reaction medium is degassed
  2. addition30 g of palladium on carbon (10%) are added
  3. customis hydrogenated at a pressure of 3 bar at 60° C
  4. filtrationThe reaction medium is filtered
  5. customevaporated off
  6. customthe residue obtained
  7. customis purified by chromatography on a silica column
  8. washeluted with a dichloromethane and methanol (99–1) mixture
  9. custom18 g (60%) of the expected product are recovered
  10. customafter evaporation of the solvents