HRID569241
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturereflux
- temperatureAfter cooling the reaction
- customwas decanted into ice water
- extractionExtraction with ether following by basification of the aqueous phase with potassium carbonate
- customyielded a semi-solid which
- extractionwas extracted with chloroform
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo to a solid
- customRecrystallization from acetonitrile
- customprovided 7.0 gm