HRID1098070
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
Potassium acetate (2.01 g, 20.50 mmol) was added to a stirred solution of 2-bromo-3-methoxy-N-(5-methylpyridin-2-yl)propanamide (Step 1) (1.40 g, 5.13 mmol) in ACN (20 mL). The reaction mixture was refluxed for 5 hrs. The reaction mixture was filtered and concentrated in vacuo. The residue was purified with column chromatography (silica gel, eluting with DCM/EtOAc:2/1) to give the title compound as a colourless solid (1.15 g), 1H NMR (300 MHz, CDCl3) δ 8.57 (br s, 1H), 8.11 (m, 2H), 7.52 (dd, 1H), 5.44 (dd, 1H), 3.89 (dd, 1H), 3.78 (dd, 1H), 3.39 (s, 3H), 2.30 (s, 3H), 2.25 (s, 3H).
WORKUP
后处理
- temperatureThe reaction mixture was refluxed for 5 hrs
- filtrationThe reaction mixture was filtered
- concentrationconcentrated in vacuo
- customThe residue was purified with column chromatography (silica gel, eluting with DCM/EtOAc:2/1)