HRID2083374

反应详情

EQUATION

反应方程式

HRID 2083374 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of n-butyl lithium in n-hexane (1.6 N, 1.6 ml) was added to 10,11-dihydro-5H-dibenzo[a,d]cycloheptene (390 mg) in anhydrous tetrahydrofuran at room temperature, and the resulting mixture was stirred under reflux for 40 minutes. A solution of 2-chloromethyl-4-isopropylmorpholine (362 mg) in benzene was added thereto while stirring under heating, and the resulting mixture was stirred under reflux for 4 hours, followed by addition of excess water. The reaction mixture was extracted with ethyl acetate. The ethyl acetate extract was dried, evaporated and chromatographed to afford 5-(4-isopropylmorpholin-2-yl)methyl-10,11-dihydro-5H-dibenzo[a,d]cycloheptene as oily material. M.P., 219° - 221° C (hydrochloride).

WORKUP

后处理

  1. temperatureunder reflux for 40 minutes
  2. stirringwhile stirring
  3. temperatureunder heating
  4. stirringthe resulting mixture was stirred
  5. temperatureunder reflux for 4 hours
  6. extractionThe reaction mixture was extracted with ethyl acetate
  7. extractionThe ethyl acetate extract
  8. customwas dried
  9. customevaporated
  10. customchromatographed