HRID1357639

反应详情

EQUATION

反应方程式

HRID 1357639 的结构方程式

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

The title compound was prepared according to the procedure of Example 20 starting from 3-thiophenemethanol (6.05 g, 53.0 mmol), K-t-BuO (0.897 g, 7.99 mmol) and 6-chloro-2-(1-piperazinyl)pyrazine (0.845 g, 4.25 mmol: obtained in Example 13, step 2). The reaction mixture was stirred at 105° C. for 7.5 h. Following chromatography on silica, solvents were evaporated off. The remaining oil was redissolved in ethyl acetetate and filtered through a short plug of alumina (5×3 cm) using ether/MeOH (96:4) as eluent. Solvent removal in vacuo gave 0.76 g (64%) of the title compound as a colorless oil. HRMS m/z for C13H16N4OS (M)+ calcd for 276.1045, found 276.1037. Anal. (C13H16N4OS.0.25 H2O) C, H, N.

WORKUP

后处理

  1. customThe title compound was prepared
  2. customwere evaporated off
  3. dissolutionThe remaining oil was redissolved in ethyl acetetate
  4. filtrationfiltered through a short plug of alumina (5×3 cm)
  5. customSolvent removal in vacuo