HRID1648220

反应详情

EQUATION

反应方程式

HRID 1648220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 25.36 g of 2-amino-5-iodobenzoic acid in 250 ml of water and 90 mL of THF was added 7.40 g of glacial acetic acid and stirred at room temperature. Then was added 7.82 g of potassium cyanate in water dropwise. Left to overnight. Added another 5.47 g of potassium cyanate. Stirred overnight. A total of 160 g of NaOH pellets were added portionwise, keeping the mixture cool in ice-water bath. The mixture was stirred at room temperature overnight. The mixture was cooled in a refrigerator and the precipitate filtered through a sintered glass funnel. The precipitate was then dissolved in water and acidified with 4N HCl. The precipitate was collected by filtration. The solid was dried in a vacuum oven to yield 25.44 g of the title compound.

WORKUP

后处理

  1. stirringStirred overnight
  2. stirringThe mixture was stirred at room temperature overnight
  3. temperatureThe mixture was cooled in a refrigerator
  4. filtrationthe precipitate filtered through a sintered glass funnel
  5. dissolutionThe precipitate was then dissolved in water
  6. filtrationThe precipitate was collected by filtration
  7. customThe solid was dried in a vacuum oven