反应详情

温度

60 °C

A 167 g. portion of 2,6-dimethoxybenzamide was slurried in 2 l. of toluene under a nitrogen atmosphere. To this solution was added 145 g. of oxalyl chloride over a one hour period. The solution was heated to 60° C. and maintained at this temperature overnight. HCl was allowed to escape while attempting to prevent water from condensing and going into the reaction mixture. Nitrogen was bubbled subsurface through a gas inlet tube while heating the reaction mixture at reflux (about 110° C.) for 11/2 hours. As stirring continued, the mixture was allowed to come to about 30° C. The solution was filtered through infusorial earth while maintaining a nitrogen atmosphere and the solvent was removed in vacuo. Yield 185 g. (97%). The oil was then stored under nitrogen.

1. additionTo this solution was added 145 g
2. temperaturemaintained at this temperature overnight
3. customfrom condensing
4. customNitrogen was bubbled subsurface through a gas inlet tube
5. temperaturewhile heating the reaction mixture
6. temperatureat reflux (about 110° C.) for 11/2 hours
7. customto come to about 30° C
8. filtrationThe solution was filtered through infusorial earth
9. temperaturewhile maintaining a nitrogen atmosphere
10. customthe solvent was removed in vacuo