反应详情

Suspend 14.8 gm of the crude alcohol from Step C in 300 ml of glacial acetic acid and heat the mixture with stirring in an oil-bath at 110°-115° C. Add 50 ml of sulfuric acid in a thin stream. Continue stirring and heating for 15 minutes. Cool and pour into 500 ml of water. Separate the solids by filtration and stir at room temperature in 125 ml of ethylacetate overnight. Separate the solids by filtration to obtain the title product. (m.p. 273°-275° C.)

1. temperatureheat the mixture
2. stirringContinue stirring
3. temperatureheating for 15 minutes
4. temperatureCool
5. customSeparate the solids
6. filtrationby filtration
7. stirringstir at room temperature in 125 ml of ethylacetate overnight
8. customSeparate the solids
9. filtrationby filtration