HRID1244263

反应详情

EQUATION

反应方程式

HRID 1244263 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

DMF (30 ml) is added to a mixture of 6-chloro-3-chloroethyl-4-propyl-pyridazine (5.01 g, 24.43 mmol), 2-fluoro-6-(imidazol-2-yl)-pyridine (3.99 g, 24.43 mmol) and anhydrous K2CO3 (10.2 g, 73.3 mmol) and the mixture is stirred at room temperature overnight. The solvent is removed in vacuo, water (30 ml) and EtOAc (30 ml) are added to the residue and the layers are separated. The aqueous layer is extracted with EtOAc (3×30 ml) and the combined extracts are washed with brine (30 ml), dried (Na2SO4) and evaporated, which provides a light brown solid. The solid is washed twice with 1:1 hexane, ether (25 ml), which provides the title compound as a light yellow solid. 1H NMR (CDCl3) 8.12–8.15 (m, 1H), 7.84 (q, 1H), 7.32 (s, 1H), 7.17 (d, 1H), 7.10 (d, 1H), 6.81–6.84 (m, 1H), 6.22 (s, 2H), 2.68 (t, 2H), 1.54–1.62 (m, 2H), 0.91 (t, 3H).

WORKUP

后处理

  1. customThe solvent is removed in vacuo, water (30 ml) and EtOAc (30 ml)
  2. additionare added to the residue
  3. customthe layers are separated
  4. extractionThe aqueous layer is extracted with EtOAc (3×30 ml)
  5. washthe combined extracts are washed with brine (30 ml)
  6. dry with materialdried (Na2SO4)
  7. customevaporated
  8. customwhich provides a light brown solid
  9. washThe solid is washed twice with 1:1 hexane, ether (25 ml), which