反应详情

1.25 g. (3.5 mmoles) of 4,4-dimethyl-9-hydroxy-7-(4-phenyl-1-methylbutyl)-1,2,3,4-tetrahydrocyclopenta[c] [1] benzopyran, 0.76 g. (3.63 mmoles) of γ-morpholinobutyric acid hydrochloride and 0.76 g. (3.70 mmoles) of dicyclohexylcarbodiimide are combined in 75 ml. of methylene chloride and stirred at room temperature for 24 hours. The insoluble by-product of dicyclohexylurea is removed by filtration and the methylene chloride solution is concentrated to 20 ml. Cyclohexane is added until the desired compound is obtained as a colorless solid. Recrystallization from methylene chloride/cyclohexane gives the desired crystalline product.

1. customThe insoluble by-product of dicyclohexylurea is removed by filtration
2. concentrationthe methylene chloride solution is concentrated to 20 ml
3. additionCyclohexane is added until the desired compound
4. customis obtained as a colorless solid
5. customRecrystallization from methylene chloride/cyclohexane
6. customgives the desired crystalline product