HRID1296649

反应详情

EQUATION

反应方程式

HRID 1296649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

K-t-BuO (0.67 g, 5.97 mmol) was added to a stirred solution of 1-(2-methoxyphenyl)ethanol (0.96 g, 6.28 mmol) in dioxane (15 mL) at 0° C. (ice-bath). After 5 min of stirring at room temperature, the reaction mixture was chilled to 0° C. (ice-bath) and 2,6-dichloropyrazine (0.78 g, 5.23 mmol) was added whereupon the reaction mixture turned yellow. After being stirrred for 35 min, dichloromethane and K2CO3 were added and the mixture was filtered. Concentration in vacuo furnished a yellow oil that was purified by silica gel chromatography (15×4 cm) using n-hexane ethyl acetate (8:2) as eluent. This gave 1.21 g (92%) of the title compound as a colorless oil. HRMS m/z calcd for C13H13ClN2O2 (M)+ 264.0666, found 264.0677. Anal. (C13H13ClN2O2) C, H, N.

WORKUP

后处理

  1. additionwas added whereupon the reaction mixture
  2. waitAfter being stirrred for 35 min
  3. filtrationthe mixture was filtered
  4. concentrationConcentration in vacuo
  5. customfurnished a yellow oil that
  6. customwas purified by silica gel chromatography (15×4 cm)