反应详情

A solution of 3.24 g (20 mmol) of 1,3-diamino-2-ethylimidazolium chloride and 16.5 g (100 mmol) of p-nitroacetophenone in 150 ml of glacial acetic acid is left to stand for 2 days, concentrated and the residue is crystallized from ethanol/ether. The crystals are placed on a column loaded with 50 g of silica gel. The material eluted with methylene chloride/methanol (7:3) is recrystallized from ethanol. There is obtained 1-amino-2-ethyl-3-[(α-methyl-p-nitrobenzylidene)amino]-imidazolium chloride of melting point 201°-203°.

1. concentrationconcentrated
2. customthe residue is crystallized from ethanol/ether
3. washThe material eluted with methylene chloride/methanol (7:3)
4. customis recrystallized from ethanol