反応 #554567

反応方程式

Phosphorus oxychloride

dimethylaniline

phenanthridine

→

9-chlorophenanthridine

収率 96.0%

溶媒

H2O

反応条件

後処理

1. 1
   温度by refluxing for 3 hours
2. 2
   抽出the obtained solid was extracted with chloroform
3. 3
   乾燥by drying with sodium sulfate
4. 4
   ろ過After filtration
5. 5
   その他the filtrate was evaporated to dryness under reduced pressure
6. 6
   その他The obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%)

実験手順

Phosphorus oxychloride (15 ml) and dimethylaniline (0.63 ml) were added to phenanthridine (2.0 g), followed by refluxing for 3 hours. The solution was poured into H2O to generate a solid, and the obtained solid was extracted with chloroform, followed by drying with sodium sulfate. After filtration, the filtrate was evaporated to dryness under reduced pressure. The obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%).

出典