HRID328326

反应详情

EQUATION

反应方程式

HRID 328326 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of 7 parts of sodamide in 90 parts of benzene maintained at 30°-35° C there is added a solution of α-phenyl-3-pyridylacetonitrile, described in U.S. Pat. No. 3,225,054 in 70 parts of benzene. The mixture is then refluxed for 1 hour, cooled and treated by portionwise addition with one equivalent of 2-morpholinoethyl chloride (J. Chem. Soc. pp 505, 1949) in 45 parts of xylene at 30°-40° C. The resulting mixture is refluxed for 2 hours, cooled, filtered and extracted with dilute hydrochloric acid. The acid extract is rendered alkaline and extracted with ether. The ether extract is treated with gaseous hydrogen chloride to yield the hydrochloride 2-phenyl-2-(3-pyridyl)-2-morpholinoethylbutyronitrile.

WORKUP

后处理

  1. temperaturemaintained at 30°-35° C
  2. temperatureThe mixture is then refluxed for 1 hour
  3. temperaturecooled
  4. customat 30°-40° C
  5. temperatureThe resulting mixture is refluxed for 2 hours
  6. temperaturecooled
  7. filtrationfiltered
  8. extractionextracted with dilute hydrochloric acid
  9. extractionThe acid extract
  10. extractionextracted with ether
  11. extractionThe ether extract
  12. additionis treated with gaseous hydrogen chloride