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
- 160 °C
PROCEDURE
实验过程
Into a dry microwave vial under N2 was added 6-Bromo-4-[1-(3-phenyl-allyl)-piperidine-4-ylamino]-chromen-2-one (20 mg, 0.046 mmol), Pd(dppf)Cl2 (about 5 mol %), and CuI (about 6 mol %) in dry THF (0.5 mL) followed by 2-ethylbutyl zinc bromide (0.273 mL, 0.138 mmol (0.5M in THF)) dropwise. The solution was heated in the microwave for 10 minutes at 160° C., filtered, and was purified by Prep HPLC to give 4.7 mg (18%) of the desired compound as the TFA salt. MS (ESI(+)Q1MS m/z 445 (M+H)+; 1H NMR (300 MHz, MeOH) δ ppm 0.90 (t, 6H), 1.29-1.38 (m, 4H), 1.60 m, 1H), 1.99 (m, 2H), 2.39 (br d, 2H), 2.60 (m, 2H), 3.24 (br t, 2H), 3.72 (br d, 2H), 3.97 (m, 3H), 5.42 (s, 1H), 6.31-6.40 (m, 1H), 6.95 (d, 1H), 7.24-7.54 (m. 8H), 7.84 (d, 1H).
WORKUP
后处理
- filtrationfiltered
- customwas purified by Prep HPLC