HRID234993

反应详情

EQUATION

反应方程式

HRID 234993 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,4-Diamino-6-methyl-5-(2,3,5-trichlorophenyl)pyrimidine (0.152 g) (Example 6) was dissolved in concentrated sulphuric acid and potassium nitrate (50 mg) was added. The solution was stirred at room temperature overnight, then poured onto ice and basified with 0.880 ammonia. The product was extracted into ethyl acetate, bulked, dried (MgSO4) and evaporated. The residue was purified by chromatography on SiO2 gel, eluting with EtOAc to 8% MeOH/EtOAc to give the desired product, 0.13 g, mp. 313°-315° C.

WORKUP

后处理

  1. extractionThe product was extracted into ethyl acetate
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customThe residue was purified by chromatography on SiO2 gel
  5. washeluting with EtOAc to 8% MeOH/EtOAc