反应详情

N-Iodosuccinamide (0.030 g, 0.13 mmol, 1.0 eq) was added to a solution of ethyl 1H-pyrrolo[3,2-c]pyridin4-ylcarbamate (0.027 g, 0.13 mmol, 1.0 eq) in THF (1 mL) at room temperature and the reaction mixture was stirred for 15 minutes. The reaction mixture was quenched with 10% NaHSO3 solution and extracted with 10/1 CHCl3/MeOH. The combined organic extracts were dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified by flash chromatography (SiO2, eluting 0-5% CHCl3/MeOH) to afford the product (0.031 g, 72%) as a solid. 1H NMR (CD3OD) δ 7.87 (d, 1H, J=5.9 Hz), 7.38 (s, 1H), 7.25 ((d, 1H, J=5.9 Hz), 4.14 (q, 2H, J=7.1 Hz), 1.12 (t, 3H, J=7.1 Hz); MS(ESI+) m/z 332 (M+H)+. Calculated: 331.9896, found: 331.9884.

1. customThe reaction mixture was quenched with 10% NaHSO3 solution
2. extractionextracted with 10/1 CHCl3/MeOH
3. dry with materialThe combined organic extracts were dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was purified by flash chromatography (SiO2, eluting 0-5% CHCl3/MeOH)