HRID394146
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
- 130 °C
PROCEDURE
实验过程
A mixture of 200 mg of 7-bromo-5-(2-chlorophenyl)-1-(2,6-dichlorophenyl)-1,6-naphthyridin-2(1H)-one (COMPOUND HHH2) and 1 mL of 4-amino-2,2,6,6-tetramethylpiperidine in 0.5 mL of DMSO was stirred at 130° C. for 3 h. The mixture was cooled, filtered, and purified by reverse-phase preparative HPLC (YMC C18 100×50 mm column; 10:90 to 90:10 v/v acetonitrile/water+0.1% TFA over 15 min; 20 mL/min) to yield the title compound. Mass spectrum (ESI) 557 (M+1). 1H NMR (500 MHz, CD3OD): selected peaks δ 1.32-1.58 (m, 14H), 2.05-2.24 (m, 2H), 4.40 (br s, 1H).
WORKUP
后处理
- temperatureThe mixture was cooled
- filtrationfiltered
- custompurified by reverse-phase preparative HPLC (YMC C18 100×50 mm column; 10:90 to 90:10 v/v acetonitrile/water+0.1% TFA over 15 min; 20 mL/min)