反应 #1994256

ord-4386054303d14f48a0b1050cf84468e6

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with methylene chloride
  2. 2
    workup.DISTILLATIONdistilled water
  3. 3
    干燥The extracted layer was dried with sodium sulfate so as to filtrate
  4. 4
    浓缩concentrate an organic solvent

实验过程

Under a nitrogen atmosphere, acridine (17.19 g, 95.92 mmol) and THF (300 ml) were introduced into a round-bottom flask. At 0° C., LiAlH4 (14.56 g, 383.66 mmol) was slowly added in halves twice thereto, followed by stirring at room temperature for 4 hours. At 0° C., the resultant product was slowly added with a sodium bicarbonate solution, and then extracted with methylene chloride and distilled water. The extracted layer was dried with sodium sulfate so as to filtrate and concentrate an organic solvent. Then, the resultant product was columned by methylene chloride and hexane (n-Hexane:MC=8:2) so as to obtain a required compound, 9,10-dihydroacridine (white solid, 14 g, 82%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08597802B2uspto-grants-2013_12