반응 #554568

반응 방정식

H2O

Benzo[b]thiophene-2-ylboronic acid

9-chlorophenanthridin

sodium carbonate

→

9-Benzothienylphenanthridine

수율 78.0%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도by refluxing under a N2 atmosphere for 5 hours
2. 2
   추출the mixture was extracted with chloroform
3. 3
   건조by drying with sodium sulfate
4. 4
   여과After filtration
5. 5
   기타the filtrate was evaporated to dryness under reduced pressure
6. 6
   기타The obtained solid was purified by column chromatography (eluent: chloroform) (amount: 1.15 g, yield: 78%)

실험 절차

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%).

출처