反应详情

To 34.0 g. (0.09 mole) of 4-(hydroxymethyl)-3,3-diphenyl-1-(1-phenylethyl)-2-pyrrolidinone in 200 ml. of chloroform was added 25.0 g. (0.20 mole) of thionylchloride. To this solution with stirring and ice bath cooling was added dropwise, 20.0 g. (0.26 mole) of dry pyridine maintaining the reaction mixture at 25° C. The solution was refluxed for 1.5 hours, concentrated in vacuo and the residue was dissolved in chloroform. The solution was washed successively with dilute hydrochloric acid solution and dilute sodium hydroxide solution. The chloroform solution was dried, filtered, and concentrated in vacuo. The residue was dissolved in hot isopropyl ether and some isooctane was added. The hot solution was decanted from a gummy residue and the product crystallized from the cooled solution. Seven grams were recrystallized in isopropyl ether to give the product which melted at 115°-120° C.

1. temperatureice bath cooling
2. additionwas added dropwise
3. customat 25° C
4. temperatureThe solution was refluxed for 1.5 hours
5. concentrationconcentrated in vacuo
6. dissolutionthe residue was dissolved in chloroform
7. washThe solution was washed successively with dilute hydrochloric acid solution and dilute sodium hydroxide solution
8. dry with materialThe chloroform solution was dried
9. filtrationfiltered
10. concentrationconcentrated in vacuo
11. dissolutionThe residue was dissolved in hot isopropyl ether
12. additionsome isooctane was added
13. customThe hot solution was decanted from a gummy residue
14. customthe product crystallized from the cooled solution
15. customSeven grams were recrystallized in isopropyl ether
16. customto give the product which melted at 115°-120° C.