反应详情

A mixture of 0.5 g (2.16 mmol) of this 4-(trifluoroacetyl)-3,4-dihydro-2H-1,4-benzoxazine, 20 ml of glacial acetic acid and 5 ml of methylene chloride was cooled to 10° in an ice bath. A solution of 1 ml of iodine monochloride in 1 ml of acetic acid was added slowly over a period of 5 minutes. Following the addition, the mixture was stirred for 45 minutes and was then diluted with water and a aqueous solution of sodium bisulfite. The product was extracted with ether. The extracts were washed with water, dried and evaporated. Crystallization of the residue from hexane yielded colorless crystals with m.p. 78°-80°.

1. temperaturewas cooled to 10° in an ice bath
2. additionthe addition
3. extractionThe product was extracted with ether
4. washThe extracts were washed with water
5. customdried
6. customevaporated
7. customCrystallization of the residue from hexane yielded colorless crystals with m.p. 78°-80°