HRID965686

反应详情

EQUATION

反应方程式

HRID 965686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-propyl-6-bromomethyl-4-chloro-pyrimidine (1 mmol), 3-fluoro-2-(1H-imidazol-2-yl)-pyridine (163 mg, 1 mmol), and K2CO3 (552 mg, 4 mmol) in DMF (6 mL) is stirred at room temperature overnight. The solvent is removed in vacuo and EtOAc (10 mL) and water (10 mL) are added to the residue. The layers are separated and the aqueous layer is extracted with EtOAc (10 mL). The combined extracts are washed with brine (10 mL), dried (Na2SO4), and evaporated. Preparative TLC separation of the residue with 5% MeOH in CH2Cl2 provides the title compound as a white solid. 1H-NMR (CDCl3) δ: 8.65 (S, 1H), 8.24 (d, 1H), 7.53 (t, 1H), 7.32 (s, 1H), 7.27-7.22 (m, 1H), 7.12 (s, 1H), 5.87 (s, 2H), 2.76 (t, 2H), 1.68-1.54 (m, 2H), 1.01 (t, 3H).

WORKUP

后处理

  1. customThe solvent is removed in vacuo and EtOAc (10 mL) and water (10 mL)
  2. additionare added to the residue
  3. customThe layers are separated
  4. extractionthe aqueous layer is extracted with EtOAc (10 mL)
  5. washThe combined extracts are washed with brine (10 mL)
  6. dry with materialdried (Na2SO4)
  7. customevaporated
  8. customPreparative TLC separation of the residue with 5% MeOH in CH2Cl2