反应详情

To a stirred suspension of compound 2a (562 mg, 1.80 mmol) in MeOH (10 mL), solid K2CO3 (0.749 g, 5.41 mmol) was added followed by dimethyl(1-diazo-2-oxopropyl)phosphonate (382 mg, 1.98 mmol) in MeOH (5 mL). The reaction was stirred at rt for 12 h and concentrated. The residue was dissolved in DCM (40 mL) and washed with water (25 mL). The aqueous layer was extracted with DCM (3×20 mL). The combined organic extracts were washed with brine (25 mL), dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was triturated with 1:1 EtOAc/heptane, filtered and dried to give compound 80a as an off-white solid. Mass Spectrum (LCMS, ESI pos.): Calcd. for C12H11BrN4O: 307.0 (M+H). found: 307.1.

1. additionwas added
2. concentrationconcentrated
3. dissolutionThe residue was dissolved in DCM (40 mL)
4. washwashed with water (25 mL)
5. extractionThe aqueous layer was extracted with DCM (3×20 mL)
6. washThe combined organic extracts were washed with brine (25 mL)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe residue was triturated with 1:1 EtOAc/heptane
11. filtrationfiltered
12. customdried