反应详情

温度

50 °C

To a stirred solution of 4-(5-chloro-2-methyl-4-nitrophenoxy)-1H-pyrazolo[3,4-b]pyridine (21.0 g, 68.9 mmol) in DMF (100 mL) was added freshly ground (mortar/pestle) potassium hydroxide (11.6 g, 207 mmol) flakes followed immediately by iodine (26.2 g, 103 mmol) under N2 at 25° C. The dark reaction was heated to 50° C. for 6 hours. The mixture was quenched by addition of aqueous 10% NaHSO3 (75 mL). The suspension was further diluted by addition of water (100 mL) and filtered. The resulting precipitate washed with water, dried by toluene azeotrope, and then left under high vacuum for 2 days. The beige powder (26.5 g, 69%) was carried forward without further purification.

1. customThe dark reaction
2. customThe mixture was quenched by addition of aqueous 10% NaHSO3 (75 mL)
3. additionThe suspension was further diluted by addition of water (100 mL)
4. filtrationfiltered
5. washThe resulting precipitate washed with water
6. dry with materialdried by toluene azeotrope
7. customThe beige powder (26.5 g, 69%) was carried forward without further purification