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
A mixture of 1.0 part of 2-amino-4-fluoro-6-fluoromethylpyrimidine, 3.0 parts of methanethiol and 50 parts of dry tetrahydrofuran was stirred at 5° C. whilst a solution of 0.16 parts of sodium in 20 parts of dry methanol was added dropwise. The temperature was kept below 10° C. with ice-bath cooling. When the addition was complete, stirring was continued for 1 hour. The resulting solution was evaporated and the residue was diluted with water and extracted three times with 50 parts of ether. The ethereal solutions were combined and dried (MgSO4). The solvent was evaporated and the crude product was purified by recrystallisation from carbon tetrachloride to give 2-amino-4-fluoromethyl-6-methylthiopyrimidine m.p. 95°-97° C.
WORKUP
后处理
- additionwas added dropwise
- customThe temperature was kept below 10° C. with ice-bath
- temperaturecooling
- additionWhen the addition
- customThe resulting solution was evaporated
- additionthe residue was diluted with water
- extractionextracted three times with 50 parts of ether
- dry with materialdried (MgSO4)
- customThe solvent was evaporated
- customthe crude product was purified by recrystallisation from carbon tetrachloride