HRID2255397

反应详情

EQUATION

反应方程式

HRID 2255397 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a flask was added 20 g. (0.1346 mole) of (2-methoxyphenyl)acetonitrile, 25 g. (0.1346 mole) of 2-(bromomethyl)tetrahydro-2H-pyran, and 200 ml. of DMSO. The mixture was stirred for five minutes at room temperature and to the resultant solution was added 22 g. (0.2692 mole) of 50% aqueous sodium hydroxide over 30 minutes with the reaction temperature being allowed to exotherm to 60° C. The reaction was stirred an additional two hours, then cooled, water added and the organic material extracted with ether. The combined ether extracts were then washed with water, dried, filtered, and the ether distilled. The organic residue wss fractionally distilled to obtain 27 g. (82% yield) of the 2-(2-methoxyphenyl)-3-(tetrahydropyran-2-yl)propionitrile boiling 145°-160° C. at 5 mm of Hg.

WORKUP

后处理

  1. additionTo a flask was added 20 g
  2. additionwas added 22 g
  3. customto exotherm to 60° C
  4. temperaturecooled
  5. extractionthe organic material extracted with ether
  6. washThe combined ether extracts were then washed with water
  7. customdried
  8. filtrationfiltered
  9. distillationthe ether distilled
  10. distillationThe organic residue wss fractionally distilled
  11. customto obtain 27 g