反应详情

Suspend sodium hydride (310 mg, 13 mmol) in a solution of ethylene glycol (800 mg, 13 mmol) in DMF (50 mL) at 0° C. After stirring for 30 min at room temperature, 7-bromo-2-chloro-quinoxaline (Preparation 26; 610 mg, 2.5 mmol) is added. Stir for 2 h at room temperature and dilute with 3:1 chloroform/isopropyl alchol. Wash the organic phase with brine and purify by FCC to give the title compound (564 mg, 85%). MS m/e (268, M+1). 1H NMR (400 MHz, CDCl3) δ 8.5 (s, 1H), 8.0 (d, J=2.0 Hz), 7.90 (dd, J=8.8, 2.0 Hz, 1H), 7.7 (d, J=8.8 Hz, 1H), 4.6 (t, d=4.8 Hz, 2H), 43.9 (t, J=4.8 Hz, 2H).

1. customat 0° C
2. stirringStir for 2 h at room temperature
3. additiondilute with 3:1 chloroform/isopropyl alchol
4. washWash the organic phase with brine
5. custompurify by FCC