HRID1724843
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
Stir a mixture of 2-chloro-7-[3-(trifluoromethyl)pyridin-2-yl]-N-[5-(trifluoromethyl) pyridin-2-yl]-[1,8]naphthyridin-4-amine (40 mg), ammonium formate (31 mg), 10% palladium on carbon (10 mg) in methanol (2 mL) at 50° C. for 2 hours. Cool, filter through Celite and evaporate to dryness. Purify by preparative thin layer chromatography, eluting with dichloromethane/methanol/ammonium hydroxide mixture to give the title compound. MS 436 (M+1). 1H NMR δ (CDCl3) 8.99 (1H, s), 8.84 (1H, d), 8.63 (1H, d), 8.61 (1H, s), 8.32 (1H, brs), 8.14 (1H, d), 8.05 (1H, brs), 7.79-7.85 (2H, m), 7.51 (1H, dd), 7.22 (1H,d).
WORKUP
后处理
- temperatureCool
- filtrationfilter through Celite
- customevaporate to dryness
- customPurify by preparative thin layer chromatography
- washeluting with dichloromethane/methanol/ammonium hydroxide mixture