HRID1763276

反应详情

EQUATION

反应方程式

HRID 1763276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 58.6 g. of 3-amino-5-(N-methylacetamido)-2,4,6-triiodobenzoic acid, 74 g. of glutaric anhydride and 8 ml. of concentrated sulfuric acid was heated on a steam bath for 5 hours. The reaction mixture was poured into water and the solid product collected by filtration. The product, consisting of 3-glutarimido-5-(N-methylacetamido)-2,4,6-triiodobenzoic acid (Example 1) was dissolved in excess dilute aqueous sodium hydroxide, and the solution warmed for thirty minutes, then cooled and 3N hydrochloric acid added slowly until precipitation was complete. The solid product was collected and recrystallized first from acetone, then from acetic acid, and finally from water to give 3'-carboxy-5'-(N-methylacetamido)-2',4',6'-triiodoglutaranilic acid, colorless prisms, m.p. 188.8°-196.0° C.

WORKUP

后处理

  1. additionA mixture of 58.6 g
  2. filtrationthe solid product collected by filtration
  3. dissolutionwas dissolved in excess dilute aqueous sodium hydroxide
  4. temperaturethe solution warmed for thirty minutes
  5. temperaturecooled
  6. addition3N hydrochloric acid added slowly until precipitation
  7. customThe solid product was collected
  8. customrecrystallized first from acetone