HRID2234630

反应详情

EQUATION

反应方程式

HRID 2234630 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 999 mg (6.44 mmol) of 2-amino-3-fluorobenzoic acid in 35 mL of water was added 500 mg (5.95 mmol) of sodium bicarbonate. The reaction was stirred and 1.77 g (6.99 mmol) of iodine was slowly added. The reaction was stirred at room temperature for 48 hours. To the solution was added an aqueous solution of sodium bisulfite and the solution was stirred vigorously for 30 minutes. The precipitate was collected by vacuum filtration and washed with water. The brown solid was dried overnight to afford 1.14 g (4.06 mmol, 63% yield) of 2-amino-3-fluoro-5-iodo-benzoic acid. 1H NMR (500 MHz, DMSO-d6) δ 7.79 (t, 1H), 7.58 (dd, 1H).

WORKUP

后处理

  1. stirringThe reaction was stirred at room temperature for 48 hours
  2. stirringthe solution was stirred vigorously for 30 minutes
  3. filtrationThe precipitate was collected by vacuum filtration
  4. washwashed with water
  5. customThe brown solid was dried overnight