HRID584892

反应详情

EQUATION

反应方程式

HRID 584892 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.4 g (3.3 mmol) of N-[4′-(2,4-dioxo-thiazolidin-5-ylidenemethyl)biphenyl-3-ylmethyl]-N-methylbenzamide, 30 ml of DMF and 25 ml of ethyl acetate are introduced into a three-necked flask. The reaction medium is degassed, 1.4 g of palladium-on-charcoal (10%) are introduced and the mixture is hydrogenated under atmospheric pressure at 60° C. The reaction medium is filtered and evaporated, and the residue obtained is purified by chromatography on a column of silica eluded with a mixture of dichloromethane and methanol (99/1). After evaporation of the solvents, 300 mg (21%) of N-[4′-(2,4-dioxo-thiazolidin-5-ylmethyl)biphenyl-3-ylmethyl]-N-methylbenzamide with a melting point of 70-71° C., are collected.

WORKUP

后处理

  1. customThe reaction medium is degassed
  2. addition1.4 g of palladium-on-charcoal (10%) are introduced
  3. customis hydrogenated under atmospheric pressure at 60° C
  4. filtrationThe reaction medium is filtered
  5. customevaporated
  6. customthe residue obtained
  7. customis purified by chromatography on a column of silica
  8. additioneluded with a mixture of dichloromethane and methanol (99/1)
  9. customAfter evaporation of the solvents, 300 mg (21%) of N-[4′-(2,4-dioxo-thiazolidin-5-ylmethyl)biphenyl-3-ylmethyl]-N-methylbenzamide with a melting point of 70-71° C.
  10. customare collected