HRID359887
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 a stirring solution of 150 mg of trifluorothymidine in 5 mL of pyridine was added a solution of 90 mg of pivaloyl chloride in 1 ml of pyridine, with cooling. Stirring was continued at room temperature for 10 hours, then the reaction mixture was poured into 20 mL of ice water and extracted with 50 mL of ethyl acetate. The extract was washed with water and dried over sodium sulfate. The ethyl acetate was removed and the residue was purified by silica gel column chromatography using 20:1 chloroform/methanol as eluent. The title compound melted at 130°-132° C. after recrystallization from a mixture of ether and n-hexane.
WORKUP
后处理
- temperaturewith cooling
- extractionextracted with 50 mL of ethyl acetate
- washThe extract was washed with water
- dry with materialdried over sodium sulfate
- customThe ethyl acetate was removed
- customthe residue was purified by silica gel column chromatography
- customThe title compound melted at 130°-132° C. after recrystallization
- additionfrom a mixture of ether and n-hexane