HRID1179869

反应详情

EQUATION

反应方程式

HRID 1179869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

At 0° C. diphosgene (0.99 g, 5.00 mmol) was added to a stirred solution of 4-trifluoromethyl-2-hydroxypyrimidine (1.64 g, 10.0 mmol) in tetrahydrofuran (25 ml). The cooling bath was removed and stirring was continued at room temperature for 1 hour. Methyl-m-tolyl-amine (0.30 g, 2.50 mmol) was added to one-fourth of the solution. After stirring overnight at room temperature the solvent was evaporated in vacuo and the residue was purified by flash column chromatography (SiO2, ethyl acetate:heptane (20:80)) followed by preparative HPLC, yielding the title compound (51 mg, 7%) as a colourless oil.

WORKUP

后处理

  1. customThe cooling bath was removed
  2. stirringAfter stirring overnight at room temperature the solvent
  3. customwas evaporated in vacuo
  4. customthe residue was purified by flash column chromatography (SiO2, ethyl acetate:heptane (20:80))