HRID1296675
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customThe title compound was prepared
- customwere evaporated off
- dissolutionThe remaining oil was redissolved in ethyl acetetate
- filtrationfiltered through a short plug of alumina (5×3 cm)
- customSolvent removal in vacuo