HRID908224

反应详情

EQUATION

反应方程式

HRID 908224 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

NaOH (3N, 0.65 ml) was added to a solution of 5-(6-bromo-2-phenyl-imidazo[1,2-a]pyridin-7-ylcarbamoyl)-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (460 mg, 0.98 mmol) in a mixture of THF (5 ml) and methanol (5 ml), and the reaction mixture was stirred at r.t. overnight. An additional amount of NaOH (3N, 0.65 ml) and water (2 ml) were added and the mixture was heated to reflux (1 h). After cooling to r.t., HCl (conc., ˜0.7 ml) was added to the cooled mixture, and the brown suspension was stirred at r.t. (15 min). The suspension was then filtered, and the precipitated title compound (150 mg, 35%) was washed with a small amount of water, dried under vacuum, and used in the next step without further purification. MS (m/e)=440.3 [M+H+].

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux (1 h)
  3. temperatureAfter cooling to r.t.
  4. stirringthe brown suspension was stirred at r.t. (15 min)
  5. filtrationThe suspension was then filtered
  6. customthe precipitated title compound (150 mg, 35%)
  7. washwas washed with a small amount of water
  8. customdried under vacuum
  9. customused in the next step without further purification