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
Compound 4o was prepared following the procedure outlined in Step 3 of Example 1 using 32 mg (0.8 mmol) of sodium hydride (60%), 86 mg (0.31 mmol) of 3-(3,4-dimethyl-benzoyl)-2,3-dihydro-1H-quinolin-4-one 3a, 3 mL of anhydrous dimethylformamide, and 101.2 mg (0.40 mmol) of 3-bromomethylpyridine hydrobromide. The crude product was purified by flash chromatography to yield 29 mg of pale yellow solid 4o: LC-MSD, m/z for C24H20N2O2, [M+H]+=369.4, [M+2H]+=370.4; Reverse phase HPLC (gradient acetonitrile 0.1% TFA 20-95% in 4 min) retention time=1.436 min; 1H NMR (400 MHz, CDCl3/HCl): δ 2.30 (d, 6H), 5.4 (s, 2H), 7.17 (d, 1H), 7.26-7.32 (m, 2H), 7.40 (t, 1H), 7.52-7.64 (m, 3H), 8.27 (s, 1H), 8.46 (d, 1H), 8.58-8.64 (m, 2H).
WORKUP
后处理
- customCompound 4o was prepared
- customThe crude product was purified by flash chromatography