反应详情

温度

60 °C

To a suspension of 5-nitrobenzo[d]oxazole-2(3H)-thione (196.2 mg, 1.0 mmol) in chloroform (10 mL) was added triethylamine (278 μL, 2 mmol) followed by 1-(bromomethyl)-4-chlorobenzene (226 mg, 1.1 mmol). The reaction was stirred at 60° C. for 2 h. After cooling, the reaction was diluted with ethyl acetate, washed with dilute aqueous hydrochloric solution and brine. The combined organic layers were dried over anhydrous MgSO4 and evaporated. The resulting solid was purified by column chromatography eluting with ethyl acetate/hexanes 1:10 v/v to afford 250 mg (78%) of the title compound (LCMS RT=7.64 min)

1. temperatureAfter cooling
2. washwashed with dilute aqueous hydrochloric solution and brine
3. dry with materialThe combined organic layers were dried over anhydrous MgSO4
4. customevaporated
5. customThe resulting solid was purified by column chromatography
6. washeluting with ethyl acetate/hexanes 1:10 v/v