反应详情

To a solution of sodium 2-methoxy-ethylate prepared by adding 7.3 g of sodium hydride (14.6 g as a state of 50% liquid paraffin dispersion) to 300 ml of methyl cellosolve, 55 g of sodium 2-chloro-5-nitrobenzenesulfonate was added with stirring. The reaction mixture was heated to a temperature from about 80° to 85° C. in a hot water bath with stirring for 30 minutes. After carried out filtration with heating, 1.5 liters of isopropyl alcohol were added to the filtrate. The crystals thus-formed were separated by filtration and washed with 100 ml of isopropyl alcohol. Yield: 59 g. m.p.: 238°-239° C.

1. additionwas added
2. temperatureThe reaction mixture was heated to a temperature from about 80° to 85° C. in a hot water bath
3. stirringwith stirring for 30 minutes
4. filtrationfiltration
5. temperaturewith heating
6. addition1.5 liters of isopropyl alcohol were added to the filtrate
7. customThe crystals thus-formed
8. customwere separated by filtration
9. washwashed with 100 ml of isopropyl alcohol