反応 #1994256

反応方程式

LiAlH4

acridine

sodium bicarbonate

→

9,10-dihydroacridine

収率 82.0%

溶媒

THF

反応条件

後処理

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

実験手順

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%).

出典