HRID1038670

反应详情

EQUATION

反应方程式

HRID 1038670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of N-(4-diethylamino-phenyl)-pyrimidine-4,6-diamine (257.4 mg, 1 mmol), 2,6-difluorophenyl isocyanate (170.6 mg, 1.1 mmol) in dry dioxane (4 mL) is shaken for 1.5 h at 80° C. After evaporation of the solvent in vacuo, the residue is distributed between CH2Cl2 and half-saturated K2CO3 solution. The organic layer is dried over Na2SO4, evaporated, and the residue purified by flash chromatography (CH2Cl2/CH3OH). The combined pure fractions are evaporated, the residue triturated with CH2Cl2 and the solid filtered off and dried in vacuo to afford the title compound.

WORKUP

后处理

  1. customAfter evaporation of the solvent in vacuo
  2. dry with materialThe organic layer is dried over Na2SO4
  3. customevaporated
  4. customthe residue purified by flash chromatography (CH2Cl2/CH3OH)
  5. customThe combined pure fractions are evaporated
  6. customthe residue triturated with CH2Cl2
  7. filtrationthe solid filtered off
  8. customdried in vacuo