HRID1249599

反应详情

EQUATION

反应方程式

HRID 1249599 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A suspension of 5-(benzyloxy)-1,4-dihydro-4-oxo-2-pyridinecarboxylic acid (8.24 g, 33.6 mmole) in 120 ml of ethanol was cooled to 0° C. and treated with a stream of dry HCl for 15 minutes. The resulting mixture was heated at 50° C. for 5.5 hours. The volatiles were removed in vacuo and the residue was treated with water. While cooling, the pH was raised to 7 with saturated potassium bicarbonate and the resulting mixture was extracted with dichloromethane. The extracts were washed with brine and dried over sodium sulfate. Filtration and concentration in vacuo produced 7.32 g of the title compound.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated at 50° C. for 5.5 hours
  2. customThe volatiles were removed in vacuo
  3. additionthe residue was treated with water
  4. temperatureWhile cooling
  5. temperaturethe pH was raised to 7 with saturated potassium bicarbonate
  6. extractionthe resulting mixture was extracted with dichloromethane
  7. washThe extracts were washed with brine
  8. dry with materialdried over sodium sulfate
  9. filtrationFiltration and concentration in vacuo