反应详情

A mixture of 2-nitrobenzaldehyde (6.8009 g), methyl 4,4-dimethoxyacetoacetate (8.7204 g), acetic acid (0.5405 g) and piperidine (0.4598 g) in benzene (30 ml) was heated to reflux for 2 hours under azeptropic dehydration. The reation mixture was diluted with benzene (100 ml), washed twice with water, and in turn with diluted aqueous sodium bicarbonate solution and water, dried over magnesium sulfate and evaporated to dryness under reduced pressure to give crude oily methyl 2-(2-nitrobenzylidene)-4,4-dimethoxyacetoacetate (15.23 g).

1. temperaturewas heated
2. temperatureto reflux for 2 hours under azeptropic dehydration
3. washwashed twice with water
4. dry with materialin turn with diluted aqueous sodium bicarbonate solution and water, dried over magnesium sulfate
5. customevaporated to dryness under reduced pressure