HRID2112610

反应详情

EQUATION

反应方程式

HRID 2112610 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of ethyl 3-cycloheptyl-3-oxo-2-(2,4,6-trifluorophenyl)propanoate (649 mg, 1.9 mmol) and 2-pyrazinecarboxamidine hydrochloride (452 mg, 2.85 mmol) in 1.5 mL of tributylamine is stirred under nitrogen atmosphere at 160° C. for 4 h. The mixture is cooled to room temperature and the excess of tributylamine is decanted off. The residue is washed with hexanes and chromatographed over silica gel, eluting with 10% methanol in ethyl acetate. Concentration provides 6-cycloheptyl-2-pyrazin-2-yl-5-(2,4,6-trifluorophenyl)pyrimidin-4-ol as a light yellow solid. MS: m/z 401.2 (M+H).

WORKUP

后处理

  1. temperatureThe mixture is cooled to room temperature
  2. customthe excess of tributylamine is decanted off
  3. washThe residue is washed with hexanes
  4. customchromatographed over silica gel
  5. washeluting with 10% methanol in ethyl acetate
  6. concentrationConcentration