反应详情

150 mg 6a was dissolved in ethanol (5.2 ml) and 2-hydrazino benzoic acid was dissolved in water (10.3 ml). These two homogenous mixtures were mixed together and stirred at room temperature for 4 hrs. Precipitation is filtered and first washed with water and then ethanol. The filtrate was put in vacuum oven for 4 hrs for complete evaporation. The mixture of 2-[N′-(6-trifluoromethyl-benzofuran-3-yl-idene)-hydrazino]-benzoic acid (120 mg), p-TsOH (1˜2 Eqv) and ethanol (5 ml) were refluxed for 30 hrs. Cooled to room temperature and evaporated in vacuo. Resulting mixture was purified by chromatography to afford compound 8 (CHCl3:MeOH=30:1).

1. additionThese two homogenous mixtures were mixed together
2. customPrecipitation
3. filtrationis filtered
4. washfirst washed with water
5. customThe filtrate was put in vacuum oven for 4 hrs for complete evaporation
6. temperaturewere refluxed for 30 hrs
7. temperatureCooled to room temperature
8. customevaporated in vacuo
9. customResulting mixture
10. customwas purified by chromatography