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 3-methylbutyl 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 6.2 mg (25%) of the desired compound as the TFA salt. MS (ESI(+)Q1MS m/z 431 (M+H)+; 1H NMR (300 MHz, MeOH) δ ppm 0.97 (d, 6H), 1.52-1.64 (m, 3H), 1.97 (br q, 2H), 2.40 (br d, 2H), 2.72 (br t, 2H), 3.23 (br t, 2H), 3.73 (d, 2H), 3.93-3.97 (m, 3H), 5.42 (s, 1H), 6.30-6.40 (m, 1H), 6.95 (d, 1H), 7.23-7.54 (m. 8H), 7.86 (d, 1H).
WORKUP
后处理
- filtrationfiltered
- customwas purified by Prep HPLC