HRID1603545

反应详情

EQUATION

反应方程式

HRID 1603545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.33 g (0.00124 mol) of (4,6-dibromopyrimidin-2-yl)-methylamine and 0.33 g (0.00248 mol) of thiophenol sodium salt were stirred in 15 ml of 1-methyl-2-pyrrolidone at 120° C. for 4 hrs. The solvent was removed and the residue was partitioned between water and diethyl ether. The ether phase was washed with sat. sodium chloride solution and dried over MgSO4. After filtration and removal of the solvent the residue was chromatographed on silica gel with diethyl ether/hexane 1:3 and subsequently dried in a high vacuum. There was obtained 0.24 g (65%) of (4-bromo-6-phenylsulphanylpyrimidin-2-yl)-methylamine as white crystals; m.p.: 122-124° C.

WORKUP

后处理

  1. customThe solvent was removed
  2. customthe residue was partitioned between water and diethyl ether
  3. washThe ether phase was washed with sat. sodium chloride solution
  4. dry with materialdried over MgSO4
  5. filtrationAfter filtration and removal of the solvent the residue
  6. customwas chromatographed on silica gel with diethyl ether/hexane 1:3
  7. customsubsequently dried in a high vacuum