反应详情

A mixture of 4-[bis(4-fluorophenyl)methyl]piperidine, 4.88 g (0.017 mole), 1-[4-(2-chloroethoxy)-3-methoxyphenyl]ethanone, 3.86 g (0.017 mole), and potassium carbonate, 5.53 g (0.04 mole) was heated overnight at gentle reflux in 350 ml of 1-butanol containing potassium iodide (0.3 g). The reaction mixture was filtered and stripped to dryness. The dark brown oil obtained was dissolvedin chloroform and extracted with 1N sulfuric acid and 5% sodium hydroxide. The chloroform layer was dried, filtered, and solvent removed. This furnished a brown oil which was subjected to flash chromatography on silica gel using hexane-ethyl acetate for elution. A white solid was obtained by evaporating the fractions containing the product. The solid was extracted with diethyl ether and the mixture was placed in the freezer overnight. A white solid was obtained which was dried at 80° C. in vacuo overnight. A yield of 2.2 g (27%) of white crystalline solid, m.p. 129°-131° C. was obtained.

1. temperaturewas heated overnight
2. filtrationThe reaction mixture was filtered
3. customThe dark brown oil obtained
4. extractionextracted with 1N sulfuric acid and 5% sodium hydroxide
5. dry with materialThe chloroform layer was dried
6. filtrationfiltered
7. customsolvent removed
8. customThis furnished a brown oil which
9. washfor elution
10. customA white solid was obtained
11. customby evaporating the fractions
12. additioncontaining the product
13. extractionThe solid was extracted with diethyl ether
14. customwas placed in the freezer overnight
15. customA white solid was obtained which
16. customwas dried at 80° C. in vacuo overnight