反应 #62193

ord-600b1aaedd034603afd57d4f4370a05a

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度at reflux for 5 h
  3. 3
    其他After removal of solvent
  4. 4
    其他the residue was purified by silica gel chromatography (2:1 hexane/EtOAc)

实验过程

A mixture of 1-((4-(Benzyloxy)phenyl)isocyanomethylsulfonyl)4-methylbenzene (4.3 g, 11.4 mmol), isonicotinaldehyde (1.34 g, 12.5 mmol) and K2CO3 (3.15 g, 22.8 mmol) in methanol (96 mL ) and DME (30 mL) was heated at reflux for 5 h. After removal of solvent, the residue was purified by silica gel chromatography (2:1 hexane/EtOAc) to provide 2.29 g (84%) of a white solid. 1H NMR (400 MHz, CDCl3) δ: 5.12v (s, 2H), 7.03 (d, 2H), 7.46 (m, 6H), 7.56 (d, 2H), 7.61 (d, 2H), 8.02 (s, 1H), 8.58 (d, 2H). MS m/z: 329 [M+1]+.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07429665B2uspto-grants-2008_09