反应详情

7.10 g. (18.7 mmoles) of 4,4-dimethyl-9-hydroxy-7-(4-p-fluorophenyl-1-methylbutyl)-1,2,3,4-tetrahydrocyclopenta [c] [1]benzopyran, prepared according to the method of Example 6, 4.33 g. (21.0 mmoles) of dicyclohexylcarbodiimide and 4.26 g. (20.3 mmoles) of γ-morpholinobutyric acid hydrochloride are combined with 325 ml. of methylene chloride and stirred at room temperature for a total of 24 hours. The insoluble by-product of dicyclohexylurea is separated by filtration and the methylene chloride is removed using a rotary evaporator. The viscous residue is dissolved in about 100 ml. of benzene and the benzene solution is filtered to remove a small amount of insoluble material. The benzene is removed using a rotary evaporator and the remaining residue is triturated with approximately 250 ml. of ether. The solid which forms is filtered, washed with ether and dried to yield a solid. The material is crystallized from benzene/ether to give the solid product.

1. customThe insoluble by-product of dicyclohexylurea is separated by filtration
2. customthe methylene chloride is removed
3. customa rotary evaporator
4. dissolutionThe viscous residue is dissolved in about 100 ml
5. filtrationof benzene and the benzene solution is filtered
6. customto remove a small amount of insoluble material
7. customThe benzene is removed
8. customa rotary evaporator
9. customthe remaining residue is triturated with approximately 250 ml
10. filtrationThe solid which forms is filtered
11. washwashed with ether
12. customdried
13. customto yield a solid
14. customThe material is crystallized from benzene/ether
15. customto give the solid product