反应详情

Methyl-4-amino-3,5-dichlorobenzoate (16.8 g, 31 mmole), 1-acetyl-2-imidazolidone (4.3 g, 33.5 mmole) in phosphoryl chloride (44 ml) were stirred at 50° C. for 3 days. After cooling the phosphoryl chloride was evaporated to give an oily residue. Iced water was added to the residue which was then basified with aqueous sodium hydroxide. The mixture was extracted with methylene chloride which was then washed with water, dried (magnesium sulphate) and evaporated to give a creamy solid. This solid was recrystallised from toluene to give the title compound (7.7 g) mp 188°-189° C.

1. customwas evaporated
2. customto give an oily residue
3. extractionThe mixture was extracted with methylene chloride which
4. washwas then washed with water
5. dry with materialdried (magnesium sulphate)
6. customevaporated
7. customto give a creamy solid
8. customThis solid was recrystallised from toluene