HRID1750314

反应详情

EQUATION

反应方程式

HRID 1750314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 5-phenyl-3-(2,2,2-trifluoroethyl)furo[2,3-d]pyrimidin-4(3H)-one (730 mg, 2.48 mmol) in DMF (10 ml) at 0° C. was added bromine (0.153 ml, 2.98 mmol). The reaction mixture was stirred at 0° C. for 1 h and then 3 h at RT. The reaction mixture was diluted with EtOAc (50 ml) and 20% w/w aq. sodium thiosulfate solution (50 ml) and the layers were separated. The organic layer was further washed with brine (2×50 ml), dried (Na2SO4) and concentrated in vacuo affording the title compound as an orange solid. LCMS RT=1.40 min, M+H+=373/375.

WORKUP

后处理

  1. custom3 h
  2. customat RT
  3. customthe layers were separated
  4. washThe organic layer was further washed with brine (2×50 ml)
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo