HRID383828

反应详情

EQUATION

反应方程式

HRID 383828 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
73 °C

PROCEDURE

实验过程

N,N-dimethyl-7-(piperazin-1-yl)benzofuran-2-carboxamide (0.09 g, 0.33 mmol) (Example 39d) was dissolved in ethanol (0.95 mL), and acetic acid (0.015 mL, 0.26 mmol) was added, followed by 2-(trifluoromethyl)-6-vinylpyridine (0.10 g, 0.58 mmol) (volatile) dissolved in ethanol (1.40 mL). The mixture was heated at 73° C. for 14 h in the microwave and then heated for another 48 h at 86° C. in an oilbath, and finally it was heated in the microwave for 15 min at 100° C. More 2-(trifluoromethyl)-6-vinylpyridine (0.10 g, 0.58 mmol) and ethanol (0.95 mL) were added and the mixture was heated in a oil bath for 7 days at 86° C. The product was purified by flash chromatography (SiO2; DCM/MeOH; gradient 0-7%) and then by preparative HPLC to give the title compound. Yield: 0.075 g (51%).

WORKUP

后处理

  1. temperatureheated for another 48 h at 86° C. in an oilbath, and finally it
  2. temperaturewas heated in the microwave for 15 min at 100° C
  3. temperaturethe mixture was heated in a oil bath for 7 days at 86° C
  4. customThe product was purified by flash chromatography (SiO2; DCM/MeOH; gradient 0-7%)