反应详情

To a DMF solution (5 mL) of NaH (0.32 g, 8 mmol) under argon, cyclohexanol (0.7 mL, 6.7 mmol) is added dropwise. The mixture is stirred at room temperature for 25 minutes, then 2-chloro-6,7-dimethoxyquinoxaline is added portionwise. The reaction is stirred for 15 minutes at room temperature, at 90° C. for 2 hours, and at 110° C. for 1 hour. The mixture is cooled, quenched with H2O, and partitioned between EtOAcl H2O. The organic layer is washed with H2O and brine, dried (MgSO4), and chromatographed (10% EtOAc/hexanes) to provide a waxy white solid (m .p. 75-78° C.). Anal. Calcd. for C21H28N2O3: C, 70.76; H, 7.92; N, 7.86; Found: C, 70.81; H, 7.79; N, 7.70.

1. stirringThe reaction is stirred for 15 minutes at room temperature, at 90° C. for 2 hours
2. waitat 110° C. for 1 hour
3. temperatureThe mixture is cooled
4. customquenched with H2O
5. custompartitioned between EtOAcl H2O
6. washThe organic layer is washed with H2O and brine
7. dry with materialdried (MgSO4)
8. customchromatographed (10% EtOAc/hexanes)
9. customto provide a waxy white solid (m .p. 75-78° C.)