反应详情

温度

79 °C

The 2-methyl-5-nitroisoindolin-1-one (50 mg, 0.26 mmol) was dissolved in EtOH (1.3 ml) with heating, and tin chloride (117 mg, 0.52 mmol) added. The solution was stirred at 79° C. for 2 hours. The mixture was cooled to RT, diluted with 4:1 water:saturated sodium bicarbonate (aq, 100 ml), extracted with EtOAc (3×100 ml), the organics combined, washed with brine, dried over Na2SO4, filtered and the volatiles removed in vacuum. The product was purified by chromatography on SiO2 eluting with 5% MeOH:DCM+1% TEA to give the titled compound.

1. temperaturewith heating
2. temperatureThe mixture was cooled to RT
3. extractionsaturated sodium bicarbonate (aq, 100 ml), extracted with EtOAc (3×100 ml)
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customthe volatiles removed in vacuum
8. customThe product was purified by chromatography on SiO2 eluting with 5% MeOH