反応 #434784

反応方程式

HCl

9-bromophenanthrene

aluminum chloride

→

dibenzo[b,k]perylene

収率 3.5%

溶媒

benzene

反応条件

後処理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   温度the mixture was heated
3. 3
   温度at reflux for one hour
4. 4
   温度to reflux for an hour
5. 5
   温度Once cooled the mixture
6. 6
   ろ過was filtered
7. 7
   洗浄The crude solid was washed with several portions of water
8. 8
   その他air-dried
9. 9
   抽出extracted with hot THF
10. 10
    その他at 300° C.

実験手順

To a stirred solution of 9-bromophenanthrene (50 g) in benzene (250 mL) was added solid aluminum chloride (50 g) gradually in portions. After the addition was complete, the mixture was heated at reflux for one hour, then cooled to ambient temperature. A slow addition of 2N HCl (250 mL) was then made (caution: exothermic). The resultant mixture was heated to reflux for an hour. Once cooled the mixture was filtered. The crude solid was washed with several portions of water and air-dried. The black solid (13.5 g) was placed in a soxhlet extractor and extracted with hot THF. The concentrated extracts were sublimed under a nitrogen flow at 300° C. and 640 mTorr to provide 1.2 g of dibenzo[b,k]perylene. The sample was pure by HPLC analysis (Keystone PAH, 5 micron, 100×3 mm).

出典