反应 #470442

ord-5820e6b389f744bfb7cce4f9c7059db1

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with ethyl acetate (3×30 mL)
  2. 2
    洗涤The combined organic layers were washed with saturated aqueous NaHCO3 and brine
  3. 3
    干燥dried over Na2SO4
  4. 4
    浓缩concentrated

实验过程

To a solution of 2-amino-5-bromopyridine (0.50 g, 2.9 mmol) in THF (10 mL) was added pyridine (343 mg, 4.3 mmol) and acetic anhydride (295 mg, 2.9 mmol) at room temperature and stirred overnight. To the mixture water (30 mL) was added, extracted with ethyl acetate (3×30 mL). The combined organic layers were washed with saturated aqueous NaHCO3 and brine, dried over Na2SO4, concentrated to give the title compound (0.58 g, 92%) as a white solid LCMS: 215 [M+2]+; 1HNMR (400 MHz, DMSO-d6) δ 2.09 (s, 3H), 7.97 (dd, J=8.8, 2.4 Hz, 1H), 8.06 (d, J=8.8 Hz, 1H), 8.41 (d, J=1.2 Hz, 1H), 10.64 (s, 1H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08367663B2uspto-grants-2013_02