反应详情

A mixture of 2.4 g. (6.06 mm.) of 5,5-dimethyl-10-hydroxy-8-(4-fluorophenyl-1-methylbutyl)-2-(2-propynyl)-1,2,3,4-tetrahydro-5H[1]benzopyrano[3,4-d]pyridine, 1.35 g. (6.06 mm.) of δ-piperidinovaleric acid hydrochloride and 1.30 g. (6.30 mm.) of dicyclohexylcarbodiimide in 100 ml. of methylene chloride are stirred at room temperature for 5 hours. The reaction mixture is cooled overnight in the refrigerator and the by-product of dicyclohexylurea removed by suction filtration. The mother liquor is evaporated and the residue dissolved in a mixture of methylene chloride/cyclohexane and allowed to stand in the cold for 2 hours. Gravity filtration separates the small amount of solid which appears, and the solvents are removed using a rotary evaporator. Crystallization from methylene chloride/diethyl ether yields the desired product.

1. additionA mixture of 2.4 g
2. temperatureThe reaction mixture is cooled overnight in the refrigerator
3. customthe by-product of dicyclohexylurea removed by suction filtration
4. customThe mother liquor is evaporated
5. dissolutionthe residue dissolved in a mixture of methylene chloride/cyclohexane
6. customcold for 2 hours
7. filtrationGravity filtration
8. customthe solvents are removed
9. customa rotary evaporator
10. customCrystallization from methylene chloride/diethyl ether