反应详情

Dry HCl gas was passed through a mixture of (4-nitrophenoxy)acetic acid 22 (100 g, 507 mmol) and ethylene glycol (300 ml) for 1 hour. During HCl gas bubbling the temperature rose to 60° C. The crude reaction mass was poured onto ice (2 kg). Crude 23 was filtered, dried and purified by column chromatography on silica gel using hexane:ethyl acetate (95:5) to give pure 23 (70 g, 57.4%) as a white powder with an m.p. between 73.5-75.5° C.

1. customDuring HCl gas bubbling the temperature
2. customrose to 60° C
3. customThe crude reaction mass
4. additionwas poured onto ice (2 kg)
5. filtrationCrude 23 was filtered
6. customdried
7. custompurified by column chromatography on silica gel