反应详情

A solution of tert-butyl 6-(2-fluoro-4-nitrophenoxy)pyrimidin-4-ylcarbamate (Compound C of Example 6, 44 mg, 0.13 mmol) in anhydrous DMF (1 mL) was cooled in an ice bath and treated with 60% NaH (44 mg, 0.16 mmol) and stirred at the same temperature for 30 minutes. The reaction mixture was treated with iodomethane (10 μL, 0.15 mmol) and stirred at 0-5° C. for 10 min. The reaction mixture was allowed to warm to room temperature and stirred for 30 min. The mixture was diluted with H2O (10 mL) and extracted with EtOAc (2×10 mL). The combined extracts were dried (MgSO4) and concentrated in vacuo to give the product (35 mg, 74%) as a pale yellow solid. 1H NMR (DMSO-d6) δ 8.57 (d, 1H, J=1.1 Hz), 8.37 (dd, 1H, J=9.8, 3.0 Hz), 8.19 (ddd, 1H, J=9.1, 2.5, 1.0 Hz), 7.71 (dd, 1H, J=8.8, 8.8 Hz), 7.66 (s, 1H), 3.38 (s, 3H), 1.51 (s, 9H).

1. stirringstirred at 0-5° C. for 10 min
2. stirringstirred for 30 min
3. extractionextracted with EtOAc (2×10 mL)
4. dry with materialThe combined extracts were dried (MgSO4)
5. concentrationconcentrated in vacuo