反应详情

To a solution of 36.5 g (0.10 mole) of α-(1-benzyl-3-pyrrolidinyl)-α,α-diphenylacetonitrile and 8.7 g (0.11 mole) of pyridine in methylene chloride was added dropwise at 25° C., 10.4 g (0.11 mole) of methyl chloroformate. The solution was refluxed for 16 hr. To the refluxing solution was added 26.1 g (0.33 mole) of pyridine and 31.2 g (0.33 mole) additional methyl chloroformate. Heating at reflux was continued for 5 hr. The mixture was cooled and washed four times with water. The methylene chloride layer was dried and concentrated in vacuo. The residual oil was crystallized twice from a mix of petroleum ether (30°-60° ) and isopropanol to give 22 g (68%) of title product, m.p. 133°-135° C.

1. temperatureThe solution was refluxed for 16 hr
2. temperatureHeating
3. temperatureat reflux
4. temperatureThe mixture was cooled
5. washwashed four times with water
6. dry with materialThe methylene chloride layer was dried
7. concentrationconcentrated in vacuo
8. customThe residual oil was crystallized twice from
9. additiona mix of petroleum ether (30°-60° ) and isopropanol