反应详情

A mixture of 3.0 g (0.01 mole) of [α,α-bis(p-fluorophenyl)]-4-piperidinemethanol, 2.3 g (0.01 mole) of N-[4-(3-chloropropoxy)phenyl]acetamide, 5.3 g (0.05 mole) of anhydrous sodium carbonate and 0.3 g of potassium iodide in 100 ml of 1-butanol gave a gum as residue. The gum was purified by column chromatography on 80 g of Florisil® and the product was eluted with 20% acetone in benzene. The combined fractions containing product were concentrated under reduced pressure to give a glass as residue. The glass was dissolved in ethyl ether, filtered through cotton, and the filtrate treated with ethereal hydrogen chloride. The resulting solid was collected by filtration, washed with ethyl ether and dried to yield 2.1 g (38%) of white solid, m.p. 135°-170° C. (with decomposition).

1. customgave a gum as residue
2. customThe gum was purified by column chromatography on 80 g of Florisil®
3. washthe product was eluted with 20% acetone in benzene
4. additionThe combined fractions containing product
5. concentrationwere concentrated under reduced pressure
6. customto give a glass as residue
7. filtrationfiltered through cotton
8. additionthe filtrate treated with ethereal hydrogen chloride
9. filtrationThe resulting solid was collected by filtration
10. washwashed with ethyl ether
11. customdried