反应详情

温度

85 °C

A solution of 200 g of phosgene in 1.6 kg of phenol was introduced at 20° C. into a 4-liter phosgenation apparatus, and 174 g of adipic acid dihydrazide were added thereto. The mixture was heated to 85° C. within one hour, with stirring; gas evolved above a reaction temperature of 45° C. Phosgene was then introduced into the reaction mixture at 85° C. over 5 hours (approx. 30 g per hour), with stirring. The solution was then purged with nitrogen at 85 to 90° C. for 30 minutes, and the major part of the phenol was finally removed by vacuum distillation at from 50 to 60° C. The remaining product was dissolved in 1 liter of toluene at 60° C. and precipitated by cooling to 20° C. The precipitate was suction filtered, washed with toluene and dried under vacuum.

1. additionwere added
2. customevolved above a reaction temperature of 45° C
3. stirringwith stirring
4. customThe solution was then purged with nitrogen at 85 to 90° C. for 30 minutes
5. customthe major part of the phenol was finally removed by vacuum distillation at from 50 to 60° C
6. dissolutionThe remaining product was dissolved in 1 liter of toluene at 60° C.
7. customprecipitated
8. temperatureby cooling to 20° C
9. filtrationfiltered
10. washwashed with toluene
11. customdried under vacuum