反应详情

To 4-methyl-7H-pyrrolo[2,3-d]pyrimidine (18, 0.634 g, 4.76 mmol) in 50 mL of dichloromethane, N-iodosuccinimide (1.3 g, 5.7 mmol) was added and the reaction stirred at room temperature for 45 minutes. The reaction was concentrated under vacuum, then ethyl acetate was added and washed with 1 N aqueous sodium thiosulfate. The organic layer was dried over sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material was purified by silica gel column chromatography, eluting with 20-100% ethyl acetate in hexane. Appropriate fractions were combined and concentrated under vacuum to provide the desired compound (19, 0.94 g). MS (ESI) [M+H+]+=260.26.

1. concentrationThe reaction was concentrated under vacuum
2. additionethyl acetate was added
3. washwashed with 1 N aqueous sodium thiosulfate
4. dry with materialThe organic layer was dried over sodium sulfate
5. filtrationfiltered
6. concentrationthe filtrate concentrated under vacuum
7. customThe resulting material was purified by silica gel column chromatography
8. washeluting with 20-100% ethyl acetate in hexane
9. concentrationconcentrated under vacuum