HRID1444117

反应详情

EQUATION

反应方程式

HRID 1444117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Dissolve 2,4,6-trichloropyrimidine (23.5 g, o.13 mol) in anhydrous MeOH (220 mL), and add solid sodium bicarbonate (28.3 g, 0.33 mol). Cool to 0° C. and add 2-methylpyrrolidine (12 g, 0.14 mol) dropwise. Let stir at room temperature for 16 h. Filter off the excess sodium bicarbonate, and evaporate under reduced pressure. Purify by SiO2 liquid chromatography, using 50:1 hexanes:EtOAc, increasing to 30:1 hexanes:EtOAc, to provide the title compound as a white solid.

WORKUP

后处理

  1. filtrationFilter off the excess sodium bicarbonate
  2. customevaporate under reduced pressure
  3. customPurify by SiO2 liquid chromatography
  4. temperatureEtOAc, increasing to 30:1 hexanes