反応 #554568

反応方程式

H2O

Benzo[b]thiophene-2-ylboronic acid

9-chlorophenanthridin

sodium carbonate

→

9-Benzothienylphenanthridine

収率 78.0%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   温度by refluxing under a N2 atmosphere for 5 hours
2. 2
   抽出the mixture 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: 1.15 g, yield: 78%)

実験手順

Benzo[b]thiophene-2-ylboronic acid (884 mg, 5.0 mmol) and 9-chlorophenanthridin (1.0 g, 4.8 mmol) were dissolved in tetrahydrofuran (30 ml), and palladium catalyst (160 mg, 0.14 mmol) and 2M sodium carbonate solution (20 ml) were added, followed by refluxing under a N2 atmosphere for 5 hours. The reaction solution was added to H2O and the mixture 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: 1.15 g, yield: 78%).

出典