HRID2264900

反应详情

EQUATION

反应方程式

HRID 2264900 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A mixture of 3-(2-fluoro-4-iodo-phenylamino)-1-methyl-1H-pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester (88 mg, 0.20 mmol), 1M aqueous sodium hydroxide solution (220 μl) and IMS (3 ml) was heated at 65° C. for 2 hours. After cooling to ambient temperature the solvent was evaporated, the resultant residue was dissolved in water and the pH of the solution was adjusted to 7 by the addition of 1N HCl solution. The precipitated solid was collected by filtration, washed with water (2 mL) then diethyl ether (2 mL) and left to air dry to provide the title compound as a yellow solid (80 mg, 92%). LCMS (method B): RT=2.11 min, M+H+=412.

WORKUP

后处理

  1. temperatureAfter cooling to ambient temperature the solvent
  2. customwas evaporated
  3. dissolutionthe resultant residue was dissolved in water
  4. additionthe pH of the solution was adjusted to 7 by the addition of 1N HCl solution
  5. filtrationThe precipitated solid was collected by filtration
  6. washwashed with water (2 mL)
  7. waitdiethyl ether (2 mL) and left to air
  8. customdry