反应详情

To 5-chloro-3-dimethylaminomethyl-pyrrolo[2,3-b]pyridine-1-carboxylic acid tert-butyl ester (141, 4.20 g, 13.6 mmol) in 100 mL of toluene, ethyl chloroformate (1.48 mL, 15.5 mmol) was added under nitrogen. The reaction was stirred at room temperature for 2 hours, then concentrated under vacuum and combined with water and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, filtered and the filtrate was concentrated under vacuum. The resulting material was purified by silica gel column chromatography eluting with 25% ethyl acetate in hexane to provide the desired compound (142, 1.60 g).

1. concentrationconcentrated under vacuum
2. extractionextracted with ethyl acetate
3. dry with materialThe organic layer was dried over sodium sulfate
4. filtrationfiltered
5. concentrationthe filtrate was concentrated under vacuum
6. customThe resulting material was purified by silica gel column chromatography
7. washeluting with 25% ethyl acetate in hexane