HRID1603546
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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
0.70 g (0.0026 mol) of (4,6-dibromopyrimidin-2-yl)-methylamine and 0.56 g (0.0026 mol) of 4-nitrothiophenol potassium salt were dissolved in 15 ml of 1-methyl-2-pyrrolidone and stirred at 50° C. for 5 hrs. The solvent was removed and the residue was partitioned in water and ethyl acetate. The combined organic phases were 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 ethyl acetate/hexane 1:9 and subsequently dried in a high vacuum. There was obtained 0.50 g (56%) of [4-bromo-6-(4-nitrophenylsulphanyl)-pyrimidin-2-yl]-methylamine as yellow crystals; m.p.: 204-205° C.
WORKUP
后处理
- customThe solvent was removed
- customthe residue was partitioned in water
- washThe combined organic phases were washed with sat. sodium chloride solution
- dry with materialdried over MgSO4
- filtrationAfter filtration and removal of the solvent the residue
- customwas chromatographed on silica gel with ethyl acetate/hexane 1:9
- customsubsequently dried in a high vacuum