反应详情

温度

100 °C

A mixture of 2.56 g (11.2 mmol) of 2-(4'-aminomethylphenyl)nitrobenzene, 2.88 g (12.2 mmol) of 4-chloro-5,6,7,8-tetrahydro-2-trifluoromethylquinazoline, and 8.0 g (58 mmol) of potassium carbonate in DMF was stirred at 100° C. overnight. The reaction mixture was quenched with water and extracted intomethylene chloride/tetrahydrofuran. The organic phase was washed with brine, dried over potassium carbonate, and purified by flash chromatography (elutions of ether/petroleum ether (1:2, then 1:1), then 10% ether/methylene chloride) to give 3.86 g (81%) of 5,6,7,8-tetrahydro-N-[(2'-nitro[1,1'-biphenyl]-4-yl)methyl]-2-(trifluoromethyl)-4-quinazolinamine, mp 150°-151° C.

1. customThe reaction mixture was quenched with water
2. extractionextracted intomethylene chloride/tetrahydrofuran
3. washThe organic phase was washed with brine
4. dry with materialdried over potassium carbonate
5. custompurified by flash chromatography (elutions of ether/petroleum ether (1:2