HRID584958

反应详情

EQUATION

反应方程式

HRID 584958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

30 g (71 mmol) of tert-butyl [4′-(2,4-dioxothiazolidin-5-ylidenemethyl)biphenyl-3-ylmethyl]methylcarbamate in 500 ml of dioxane are placed in a reactor. The reaction medium is degassed, followed by addition of g (1 equivalent by mass) of 10% palladium-on-charcoal. The system is placed under 3 bar of hydrogen and heated at 50° C. for seven hours. The reaction medium is filtered through Celite and evaporated, and the residue obtained is purified by chromatography on a column of silica with an fluent mixture of dichloromethane and methanol (98/2). After evaporation of the solvents, 18 g (60%) of the expected product are collected.

WORKUP

后处理

  1. customThe reaction medium is degassed
  2. filtrationThe reaction medium is filtered through Celite
  3. customevaporated
  4. customthe residue obtained
  5. customis purified by chromatography on a column of silica with an fluent mixture of dichloromethane and methanol (98/2)
  6. customAfter evaporation of the solvents, 18 g (60%) of the expected product
  7. customare collected