HRID569241

反应详情

EQUATION

反应方程式

HRID 569241 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To. 22.0 gm of 5-(3-methoxyphenyl)-1-phenyl-4-(p-toluenesulfonyloxymethyl)pyrrolidin-2-one in 150 ml. of dimethylformamide was added 21 ml. of 40% aqueous dimethylamine, the solution refluxed for 3 hours and then 21 ml. more of 40% aqueous dimethylamine added and reflux continued for an additional 3 hours. After cooling the reaction was decanted into ice water and acidified. Extraction with ether following by basification of the aqueous phase with potassium carbonate yielded a semi-solid which was extracted with chloroform, dried (Na2SO4), filtered and concentrated in vacuo to a solid. Recrystallization from acetonitrile provided 7.0 gm. of beige crystals, m.p. 88°-92°.

WORKUP

后处理

  1. temperaturereflux
  2. temperatureAfter cooling the reaction
  3. customwas decanted into ice water
  4. extractionExtraction with ether following by basification of the aqueous phase with potassium carbonate
  5. customyielded a semi-solid which
  6. extractionwas extracted with chloroform
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo to a solid
  10. customRecrystallization from acetonitrile
  11. customprovided 7.0 gm