HRID621864

反应详情

EQUATION

反应方程式

HRID 621864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-(3-chlorophenyl)-3H-imidazo[4,5-b]pyridine-3-acetic acid ethyl ester (6.0 g, 0.019 mole), sodium hydroxide pellets (0.9 g, 0.023 mole), and 50 ml of ethanol-water (2:1) was refluxed for 1 hour. The reaction mixture was cooled and the ethanol evaporated in vacuo. The residual aqueous mixture was diluted with water (40 ml) and extracted with diethyl ether (2×25 ml). The aqueous portion was acidified with concentrated hydrochloric acid to a pH of 5-6. After precipitation was complete, the solid was collected by filtration, giving 5.9 g (100%). Recrystallization from ethanol gave 4.7 g of cream colored needles, mp 214°-216° C.

WORKUP

后处理

  1. temperaturewas refluxed for 1 hour
  2. temperatureThe reaction mixture was cooled
  3. customthe ethanol evaporated in vacuo
  4. additionThe residual aqueous mixture was diluted with water (40 ml)
  5. extractionextracted with diethyl ether (2×25 ml)
  6. customAfter precipitation
  7. filtrationthe solid was collected by filtration
  8. customgiving 5.9 g (100%)
  9. customRecrystallization from ethanol
  10. customgave 4.7 g of cream colored needles, mp 214°-216° C.