HRID1592971
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe reaction medium is degassed
- addition30 g of palladium on carbon (10%) are added
- customis hydrogenated at a pressure of 3 bar at 60° C
- filtrationThe reaction medium is filtered
- customevaporated off
- customthe residue obtained
- customis purified by chromatography on a silica column
- washeluted with a dichloromethane and methanol (99-1) mixture
- custom18 g (60%) of the expected product are recovered
- customafter evaporation of the solvents