HRID386540

反应详情

EQUATION

反应方程式

HRID 386540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a stirring solution of piperidin-4-ol (2.33 g, 23.0 mmol, Aldrich) and potassium carbonate (6.36 g, 46.0 mmol, EMD) in DMF (15 mL) at room temperature was added 2-chloro-5-propylpyrimidine (4.33 g, 27.6 mmol, Wako). The reaction mixture was heated at 100° C. for 3 h then diluted with H2O. The resulting mixture was extracted with EtOAc (2×). The organic layers were combined, dried over Na2SO4 and concentrated in vacuo to a brown oil. The oil was purified by flash chromatography (SiO2, 0 to 100% EtOAc in CH2Cl2) to yield 5.01 g of desired product as a white solid. MS (ESI) 222 (M+H).

WORKUP

后处理

  1. extractionThe resulting mixture was extracted with EtOAc (2×)
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo to a brown oil
  4. customThe oil was purified by flash chromatography (SiO2, 0 to 100% EtOAc in CH2Cl2)