反应 #1885090

ord-e717c0726c094481aedb1d775f3cba45

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他To the cooled reaction mixture
  2. 2
    其他the product was obtained
  3. 3
    萃取by extracting with methylene chloride
  4. 4
    干燥dried over sodium sulfate
  5. 5
    浓缩concentrated in vacuo

实验过程

A suspension of 6,7-difluoro-4-hydroxy quinoline 2i was refluxed with phosphorus oxychloride for 30 minutes. To the cooled reaction mixture was added aqueous ammonia and the product was obtained by extracting with methylene chloride, dried over sodium sulfate and concentrated in vacuo. 1H NMR (CDCl3) δ (ppm): 1.44 (3H, t, J=7.14 Hz), 2.70 (3H, s), 4.50 (2H, q, J=7.14 Hz), 7.62 (1H, t, J=7.69 Hz), 7.78 (1H, dd, J=10.71, 7.69 Hz), 7.95 (2H, d, J=10.72, 8.24 Hz). m/z 286.7 (MH+).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08343957B2uspto-grants-2013_01