HRID1500683

反应详情

EQUATION

反应方程式

HRID 1500683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 5-(2-fluoro-4-cyclopropylphenylamino)-imidazo[1,5-a]pyridine-6-carboxylic acid methyl ester (573 mg, 1.73 mmol) in methanol (20 mL) was added aqueous sodium hydroxide (10 mL, 1M, 10 mmol) and the reaction mixture stirred at 70° C. for 30 minutes. The reaction mixture was concentrated in vacuo to −20 mL volume and the resultant solution diluted with water (20 mL) and filtered. The filtrate was acidified to pH 1 by addition of aqueous hydrochloric acid (1M) causing a precipitate to form. The precipitate was collected by filtration and dried under vacuum at 45° C. to yield the title compound as a dark tan solid (476 mg, 87%). LCMS (Method B): RT=2.81 min, M+H+=318.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo to −20 mL volume
  2. additionthe resultant solution diluted with water (20 mL)
  3. filtrationfiltered
  4. additionThe filtrate was acidified to pH 1 by addition of aqueous hydrochloric acid (1M)
  5. customto form
  6. filtrationThe precipitate was collected by filtration
  7. customdried under vacuum at 45° C.