反应详情

温度

0 °C

To a solution of (1Z,2E)-N′-hydroxy-3-(4-((E)-2-phenyl-1-(1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-5-yl)but-1-en-1-yl)phenyl)acrylimidamide (51 mg, 0.1 mmol) in anhydrous DMF (0.4 mL) was added 2-ethylhexylchloroformate (20 μL, 0.1 mmol) followed by pyridine (9 μL, 0.11 mmol). The reaction mixture was stirred at 0° C. for 1 h and then partitioned between water and EtOAc. The aqueous layer was extracted with EtOAc (2×), and the combined organics were dried over MgSO4 and concentrated. The residue was dissolved in xylenes (1 mL), heated at 130° C. for 2 h, and then concentrated to afford 25 mg of the title compound. LCMS: 519 (M+H)+.

1. custompartitioned between water and EtOAc
2. extractionThe aqueous layer was extracted with EtOAc (2×)
3. dry with materialthe combined organics were dried over MgSO4
4. concentrationconcentrated
5. dissolutionThe residue was dissolved in xylenes (1 mL)
6. temperatureheated at 130° C. for 2 h
7. concentrationconcentrated