反应详情

2-Bromoacetyl chloride (9.7 g) is added dropwise to a stirred mixture of 3,4-dihydro-4-methyl-2(1H)-quinazolinone (5 g), anhydrous aluminum chloride (10.3 g) and carbon disulfide (100 ml) under nitrogen. The reaction mixture is refluxed for about 18 hours, the carbon disulfide decanted, and the residue treated with hydrochloric acid (6N) and ethyl acetate. The layers are separated, and the aqueous layer extracted with ethyl acetate and the combined ethyl acetate extracts washed with sat'd. aqueous sodium bicarbonate and water and dried. The dried organic extract is filtered and the filtrate evaporated, affording the desired product as a solid, which is used without further purification, M.P. 188°-190° C.

1. temperatureThe reaction mixture is refluxed for about 18 hours
2. customthe carbon disulfide decanted
3. additionthe residue treated with hydrochloric acid (6N) and ethyl acetate
4. customThe layers are separated
5. extractionthe aqueous layer extracted with ethyl acetate
6. washthe combined ethyl acetate extracts washed with sat'd
7. dry with materialaqueous sodium bicarbonate and water and dried
8. extractionThe dried organic extract
9. filtrationis filtered
10. customthe filtrate evaporated