HRID865328

反应详情

EQUATION

反应方程式

HRID 865328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mechanically stirred solution of 26.3 grams of 5-iodo-2-amino benzoic acid (0.1 mol), 10.6 grams of sodium carbonate (0.1 mol), and 250 mL water, cooled to 0° C., was slowly added, via an addition funnel, 80 mL of a 1.93M solution of phosgene in toluene. After 2 hours, the precipitated product was isolated by filtration. The solids were washed with 200 mL water, 300 mL of a 1:1 mixture ethanol and ether, 200 mL of ether, and dried under vacuum to yield 24.3 grams (84%) of 5-iodoisatoic anhydride (264°-268° C., decomposition).

WORKUP

后处理

  1. additionwas slowly added, via an addition funnel
  2. customthe precipitated product was isolated by filtration
  3. washThe solids were washed with 200 mL water, 300 mL of a 1:1 mixture ethanol and ether, 200 mL of ether
  4. customdried under vacuum