反应 #1753629

ord-72680a9d426c4542a193403c708915a5

溶剂

反应条件

温度
110°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The reaction mixture was quenched with water
  2. 2
    萃取extracted with EtOAc three times
  3. 3
    萃取The organic extract
  4. 4
    洗涤was washed with water and brine
  5. 5
    干燥dried over sodium sulfate
  6. 6
    浓缩concentrated under reduced pressure

实验过程

To a solution of 5-bromo-2-methylphenol (1.0 g, 0.005 mol) in DMF (10 mL) was added K2CO3 (1.38 g, 0.01 mol) at RT. 2-Chloro-5-(trifluoromethyl)pyridine (908 mg, 0.005 mol) was added and the reaction was refluxed at 110° C. for 12 h. The reaction mixture was quenched with water and extracted with EtOAc three times. The organic extract was washed with water and brine, dried over sodium sulfate and concentrated under reduced pressure to give the title compound (1.5 g, 88%). 1H NMR (500 MHz, CDCl3): δ 8.42 (s, 1H), 7.92 (d, J=2.15 Hz, 1H), 7.32 (t, J=6.45 1H), 7.23 (d, J=1.5 Hz, 1H), 7.17 (d, J=8.05 Hz, 1H), 7.03 (d, J=8.65 Hz, 1H), 2.12 (s, 3H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08044052B2uspto-grants-2011_10