反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent is removed in vacuo, water (30 ml) and EtOAc (30 ml)
- additionare added to the residue
- customthe layers are separated
- extractionThe aqueous layer is extracted with EtOAc (3×30 ml)
- washthe combined extracts are washed with brine (30 ml)
- dry with materialdried (Na2SO4)
- customevaporated
- customwhich provides a light brown solid
- washThe solid is washed twice with 1:1 hexane, ether (25 ml), which