HRID127509

反应详情

EQUATION

反应方程式

HRID 127509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The product of the above (2) (13.2 g) is dissolved in a mixture of ethanol (300 ml) and triethylamine (20 ml). The solution is refluxed for 1 hour and further 2 hours after addition of a solution of potassium cyanate (25 g) in a mixture of ethanol (170 ml) and water (80 ml) and evaporated to remove the solvent. The residue is extracted with ether after addition of water. The extract is washed with water, dried and evaporated to remove the solvent. The oily residue (15 g) is chromatographed on an column of silica gel (450 g) and eluted with benzene. The eluate is condensed to give the title compound as crystals melting at 125°-126° C. Yield: 69%

WORKUP

后处理

  1. temperatureThe solution is refluxed for 1 hour and further 2 hours
  2. customevaporated
  3. customto remove the solvent
  4. extractionThe residue is extracted with ether
  5. additionafter addition of water
  6. washThe extract is washed with water
  7. customdried
  8. customevaporated
  9. customto remove the solvent
  10. customThe oily residue (15 g) is chromatographed on an column of silica gel (450 g)
  11. washeluted with benzene
  12. customcondensed