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
CONDITIONS
反应条件
- 温度
- -78 °C
PROCEDURE
实验过程
BuLi (0.875 mL, 1.40 mmol, 1 M solution in THF) was added slowly to a solution of furan (0.106 mL, 1.45 mmol) in THF (2 mL) at −78° C., and the mixture was stirred at −78° C. for 1 h. A solution of 1-{[2-(2-chlorophenyl)-1-(4-chlorophenyl)-1H-imidazol-4-yl]carbonyl}-4-piperidinone (0.3 g, 0.68 mmol) in THF (1 mL) was added slowly. The mixture was stirred at −78° C. for 2 h and saturated NH4Cl (3 mL) and water added. The mixture was extracted with ethyl acetate (3×20 mL) and dried over MgSO4. The product (0.142 g, 61%) was isolated by column (ethyl acetate). MS (Electrospray) 482 (M)+; 1H NMR (300 MHz, CD2Cl2) δ .7.85 (s, 1H), 7.51-7.31 (m, 7H), 7.10-6.98 (m, 4H), 7.17-7.10 (m, 2H), 6.39 (s, 1H), 6.29 (s, 1H), 4.68 (br, 1H), 4.28 (br, 1H), 3.94 (br, 1H), 3.57 (br, 1H), 2.26-1.91 (m, 4H).
WORKUP
后处理
- stirringThe mixture was stirred at −78° C. for 2 h
- extractionThe mixture was extracted with ethyl acetate (3×20 mL)
- dry with materialdried over MgSO4