反应详情

温度

150 °C

A mixture of 4-chloro-1H-pyrrolo[2,3-b]pyridine (Step B, 1.0 g, 6.5 mmol) and 3,4-dinitrophenol (1.41 g, 7.6 mmol) was heated at 150° C. for 8 h. The resulting crude solid was dissolved in NaOH (12N) and CH2Cl2. The aqueous layer was extracted several times with CH2Cl2. The insoluble material was solubilized in acetone. The acetone solution was diluted with CH2Cl2 and washed with water. The combined CH2Cl2 layers were dried and concentrated under vacuum. The crude material was purified on silica gel using a CH2Cl2/EtOH gradient (100/0 to 90/10) to give 4-(3,4-dinitro-phenoxy)-1H-pyrrolo[2,3-b]pyridine.

1. extractionThe aqueous layer was extracted several times with CH2Cl2
2. additionThe acetone solution was diluted with CH2Cl2
3. washwashed with water
4. dry with materialThe combined CH2Cl2 layers were dried
5. concentrationconcentrated under vacuum
6. customThe crude material was purified on silica gel using a CH2Cl2/EtOH gradient (100/0 to 90/10)