反应详情

A mixture of 2-(4-hydroxy-3-nitrobenzylidene)acetylacetone (40 g), benzamidine hydrochloride (30.2 g) and triethylamine (31.2 ml) in n-butanol (400 ml) was refluxed for 2 hours. The reaction mixture, added ethyl acetate (100 ml), was washed with water (200 ml) and 5% hydrochloric acid (200 ml) successively. The solvent was evaporated and the residue was stirred with ethyl acetate (200 ml) for 1 hour. The crystals were collected by filtration, added a mixture of chloroform (200 ml) and water (200 ml) and adjusted to pH 8.5 by saturated potassium carbonate. The organic layer was evaporated in vacuo to give crude 5-acetyl-1,6-dihydro-6-(4-hydroxy-3-nitrophenyl)-4-methyl-2-phenylpyrmidine (45.5 g).

1. temperaturewas refluxed for 2 hours
2. washwas washed with water (200 ml) and 5% hydrochloric acid (200 ml) successively
3. customThe solvent was evaporated
4. filtrationThe crystals were collected by filtration
5. additionadded
6. additiona mixture of chloroform (200 ml) and water (200 ml)
7. customThe organic layer was evaporated in vacuo