HRID345349

反应详情

EQUATION

反应方程式

HRID 345349 的结构方程式

PROCEDURE

实验过程

A solution of 21.7 g of 4-(tert-butyl-dimethylsilyloxymethyl)-2-cyanopyridine in 220 ml anhydrous ethanol containing 0.2 g of sodium is stirred at room temperature for 18 hours, cooled to 0° and 22 ml 6N hydrochloric acid is then added. The solution is stirred at room temperature for 18 hours cooled to 0°, 7.5 ml 6N sodium hydroxide added followed by 20 ml saturated aqueous sodium carbonate. Extraction with methylene chloride, then drying, filtering and concentrating the extract yields an oil which crystallizes from ether to yield ethyl 4-(hydroxymethyl)-pyridine-2-carboxylate.

WORKUP

后处理

  1. temperaturecooled to 0°
  2. temperaturecooled to 0°
  3. extractionExtraction with methylene chloride
  4. customdrying
  5. filtrationfiltering
  6. concentrationconcentrating the extract
  7. customyields an oil which
  8. customcrystallizes from ether