反应详情

温度

0 °C

Into a 250 mL 3-necked round bottom flask was placed dichloromethane (30 mL). To the mixture was added mCPBA (m-chloroperbenzoic acid) (2.78 g, 13.69 mmol), while cooling to a temperature of 0° C. This was followed by the addition of a solution of 1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine-3-carbaldehyde (3 g, 10.49 mmol) in dichloromethane (100 mL), which was added dropwise with stirring, while cooling to a temperature of 0° C. The resulting solution was allowed to react, with stirring, 2 hours while the temperature was maintained at 0° C. Then the resulting solution was allowed to react, with stirring, overnight while the temperature was maintained at 30° C. in a bath of oil. The reaction progress was monitored by LC-MS. The residue was purified by eluting through a column with a 1:10 ethyl acetate/petroleum ether solvent system. This resulted in 2 g (63%) of 1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridin-3-yl formate as a light yellow solid.

1. customInto a 250 mL 3-necked round bottom flask was placed
2. additionwas added dropwise
3. temperaturewhile cooling to a temperature of 0° C
4. customto react
5. stirringwith stirring, 2 hours while the temperature
6. temperaturewas maintained at 0° C
7. customto react
8. stirringwith stirring, overnight while the temperature
9. temperaturewas maintained at 30° C. in a bath of oil
10. customThe residue was purified
11. washby eluting through a column with a 1:10 ethyl acetate/petroleum ether solvent system
12. customThis resulted in 2 g (63%) of 1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridin-3-yl formate as a light yellow solid