HRID3912

反应详情

EQUATION

反应方程式

HRID 3912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added dropwise
  2. customThe temperature was kept below 10° C. with ice-bath
  3. temperaturecooling
  4. additionWhen the addition
  5. customThe resulting solution was evaporated
  6. additionthe residue was diluted with water
  7. extractionextracted three times with 50 parts of ether
  8. dry with materialdried (MgSO4)
  9. customThe solvent was evaporated
  10. customthe crude product was purified by recrystallisation from carbon tetrachloride