反应详情

温度

0 °C

3-(1H-Pyrrolo[2,3-b]pyridin-5-yl)-azetidine-1-carboxylic acid tert-butyl ester (56 mg, 0.2 mmol) was dissolved in DMA (2 ml) and cooled to 0° C. Sodium hydride (16 mg, 0.37 mmol, 55%) was added, and the reaction mixture was stirred for 30 minutes at 0° C. Benzenesulfonyl chloride (40 μl, 0.29 mmol) was added slowly to the reaction mixture. Stirring was continued for 3 hours. Water and ethyl acetate was added to the reaction mixture. The organic phase was extract three times with water. The organic phase was dried over magnesium sulphate, filtered, and the solvent was evaporated under reduced pressure. The residue was purified by column chromatography on silica gel (ethylacetate:cylcohexane) to afford the title compound (10 mg, 12% yield).

1. stirringStirring
2. waitwas continued for 3 hours
3. extractionThe organic phase was extract three times with water
4. dry with materialThe organic phase was dried over magnesium sulphate
5. filtrationfiltered
6. customthe solvent was evaporated under reduced pressure
7. customThe residue was purified by column chromatography on silica gel (ethylacetate:cylcohexane)