反応 #2006423

ord-e3f84e9606f34caa918071ab9352a4be

反応方程式

C=Cc1ccc(C(=O)O)cc1
4-vinyl-benzoic acid
Sc1ccccc1
benzenethiol
CC(C)(C#N)N=NC(C)(C)C#N
VAZO
CCc1cc(-c2cccs2)ccc1C(=O)O
white solid
収率 85.0%
CCc1cc(-c2cccs2)ccc1C(=O)O
4-(2-Thiophenyl)-ethyl Benzoic Acid
収率 85.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他According to the published procedure (Gareau et al., Tet. Lett., 1994, 1837), under nitrogen atmosphere in a 50 mL round bottomed flask
  2. 2
    温度at reflux
  3. 3
    その他the solvent was evaporated under vacuo
  4. 4
    その他The solid was purified by trituration

実験手順

According to the published procedure (Gareau et al., Tet. Lett., 1994, 1837), under nitrogen atmosphere in a 50 mL round bottomed flask containing 4-vinyl-benzoic acid (1.0 g, 6.75 mmoles) in 10 mL of benzene (0.7 M) was added benzenethiol (797 μL, 7.76 mmoles) followed by VAZO™ (Aldrich Chemical Company, 495 mg, 2.02 mmoles). The mixture was stirred for 12 hours at reflux. The resulting solution was cooled at room temperature and the solvent was evaporated under vacuo. The solid was purified by trituration using hexane and dichloromethane to afford 1.94 g (85%) of white solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: USRE043343E1uspto-grants-2012_05