HRID1290748

反应详情

EQUATION

反应方程式

HRID 1290748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 0.4 g of 10-benzylidene-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazin-4-one, 90 ml of dimethylformamide and 10 ml of methanol is hydrogenated at a temperature in the region of 20° C. at a pressure of 1.9 bar of hydrogen for 3 hours in the presence of 10% palladium on charcoal. The catalyst is then filtered off under inert atmosphere and the solvents are evaporated off. The brown solid obtained (0.37 g) is purified by chromatography on a column of silica (35 g) with a mixture of dichloromethane and methanol (90/10 by volume). After trituration with 5 ml of dichloromethane, filtration and drying at 100° C., 0.15 g of 10-benzyl-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazin-4-one is obtained, in the form of a beige solid melting above 260° C. (Analysis % calculated C: 76.66, H: 4.82, N: 13.41, O: 5.11, % found C: 76.3, H: 4.6, N: 13.4).

WORKUP

后处理

  1. filtrationThe catalyst is then filtered off under inert atmosphere
  2. customthe solvents are evaporated off
  3. customThe brown solid obtained (0.37 g)
  4. customis purified by chromatography on a column of silica (35 g) with a mixture of dichloromethane and methanol (90/10 by volume)
  5. filtrationAfter trituration with 5 ml of dichloromethane, filtration
  6. customdrying at 100° C.