HRID268314

反应详情

EQUATION

反应方程式

HRID 268314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 100 ml. flask was charged with 2.0 g. 2-carbamylnicotinic acid* suspended in 20 ml. dimethylformamide. A 5.5 g. portion of lead tetra-acetate was added to the suspension, and the mixture was stirred at 50°-60° for 1 hour. The reaction mixture was poured into 20 ml. water; solids were separated by filtration, and 3-azaisatoic anhydride was recrystallized from dioxane, and dried in vacuo for 2 hours. The final yield of 3-azaisatoic anhydride amounted to 1.48 g., melting point 217°-219°, and represented 75 percent of theory. The structure was confirmed by elemental analysis and infrared spectroscopy.

WORKUP

后处理

  1. additionflask was charged with 2.0 g
  2. additionThe reaction mixture was poured into 20 ml
  3. customsolids were separated by filtration, and 3-azaisatoic anhydride
  4. customwas recrystallized from dioxane
  5. customdried in vacuo for 2 hours