HRID1921909

反应详情

EQUATION

反应方程式

HRID 1921909 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

2-Pyridin-4-yl-pyrimidin-4-ol (200 mg, 1.16 mmol) was suspended in DCE (10 mL) then POBr3 (497 mg, 1.73 mmol) was added in one portion. The reaction mixture was heated to 95° C. (bath) for 18 h then cooled to 20° C. H2O (30 mL) and CH2Cl2 (30 mL) were added, then the biphasic mixture was stirred vigorously for 30 min. The layers were separated and the aqueous phase was extracted with CH2Cl2 (3×30 mL). The combined organics were evaporated to dryness to afford the title compound: m/z (ES+)=236, 238 (1:1) [M+H]+.

WORKUP

后处理

  1. temperaturethen cooled to 20° C
  2. customThe layers were separated
  3. extractionthe aqueous phase was extracted with CH2Cl2 (3×30 mL)
  4. customThe combined organics were evaporated to dryness