HRID1921909
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethen cooled to 20° C
- customThe layers were separated
- extractionthe aqueous phase was extracted with CH2Cl2 (3×30 mL)
- customThe combined organics were evaporated to dryness