HRID472925

反应详情

EQUATION

反应方程式

HRID 472925 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.51 ml (1.51 mmol) of a 1N aqueous sodium hydroxide solution are added to 300 mg (0.92 mmol) of methyl 3-(4-amino-3-methoxybenzoyl)imidazo[1,5-a]pyridine-6-carboxylate obtained in example 83 in 15 ml of a mixture (5/5/5) of dioxane, dichloromethane and methanol. The reaction medium is stirred at ambient temperature overnight and then concentrated under reduced pressure. The residue is dissolved in water, washing is carried out with ethyl acetate and then the aqueous phase is acidified with 1.5 ml of 1N hydrochloric acid. The precipitate formed is filtered off, washed with water and then dried. 346 mg of a yellow solid are collected, which solid is salified in the sodium salt.0.7H2O form. Melting point: 306° C.; 1H NMR (d6-DMSO): 3.87 (3H, s), 6.72 (1H, d), 7.70-7.78 (3H, m), 7.96 (1H, s), 8.18 (1H, d), 10.09 (1H, s)

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. dissolutionThe residue is dissolved in water
  3. washwashing
  4. customThe precipitate formed
  5. filtrationis filtered off
  6. washwashed with water
  7. customdried
  8. custom346 mg of a yellow solid are collected
  9. customform