HRID1500678

反应详情

EQUATION

反应方程式

HRID 1500678 的结构方程式

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a solution of 5-(2-fluoro-4-iodophenylamino)-imidazo[1,5-a]pyridine-6-carboxylic acid methyl ester (5.6 g, 13.6 mmol) in IMS (50 mL) was added aqueous sodium hydroxide (27.2 mL, 1M, 27.2 mmol) and the reaction mixture stirred at 65° C. for 2 hours. The reaction mixture was concentrated in vacuo to remove the IMS. The resultant solution was acidified to pH ˜5 by addition of aqueous hydrochloric acid (1M) causing a precipitate to form. The product was collected by filtration and dried under vacuum at 45° C. to yield the title compound as a beige solid (5.4 g, 100%). LCMS (Method B): RT=2.79 min, M+H+=398.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customto remove the IMS
  3. additionThe resultant solution was acidified to pH ˜5 by addition of aqueous hydrochloric acid (1M)
  4. customto form
  5. filtrationThe product was collected by filtration
  6. customdried under vacuum at 45° C.