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
Experimental conditions analogous to those described for Step 2 of Example 1 were used with 69 mg (0.224 mmol) of 3-(3,4-Dimethyl-benzoyl)-6,7-dimethyl-1H-[1,8]naphthyridin-4-one, 11 mg (0.269 mmol, 60% dispersion in oil) of sodium hydride, 67.5 mg (0.269 mmol) of 2-bromo-6-bromomethyl-pyridine and 2.0 mL of N,N dimethylformamide. The crude brown solid was purified by flash column chromatography using 30-100% ethyl acetate in hexane to yield 1-(6-Bromo-pyridin-2-ylmethyl)-3-(3,4-dimethyl-benzoyl)-6,7-dimethyl-1H-[1,8]naphthyridin-4-one as an off white solid. LC-MSD, m/z for C25H22BrN3O2 [M+H]: 476.09 LC retention time on HPLC, C18 column gradient 20-95% acetonitrile with 0.1% TFA in 4 minutes: 2.8 min
WORKUP
后处理
- customThe crude brown solid was purified by flash column chromatography