反応 #84282

ord-2f427f502f364bb1a8fb17ec4914a72e

反応方程式

CCON=C(CNC(=O)c1ccccc1C(F)(F)F)c1ncc(C(F)(F)F)cc1Cl
N-[2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-2-(ethoxyimino)ethyl]-2-(trifluoromethyl)benzamide
O=C(c1ccccc1)c1ccccc1
benzophenone
CCO/N=C(/CNC(=O)c1ccccc1C(F)(F)F)c1ncc(C(F)(F)F)cc1Cl
desired product
収率 87.5%
CCO/N=C(/CNC(=O)c1ccccc1C(F)(F)F)c1ncc(C(F)(F)F)cc1Cl
(Z)—N-[2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-2-(ethoxyimino)ethyl]-2-(trifluoromethyl)benzamide
収率 87.5%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他After completion of the reaction
  2. 2
    その他the solvent was evaporated under reduced pressure
  3. 3
    その他the resulting residue was purified by silica gel column chromatography

実験手順

To 48 mg of N-[2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-2-(ethoxyimino)ethyl]-2-(trifluoromethyl)benzamide in 3 ml of acetonitrile, 1 mg of benzophenone was added, and the mixture was irradiated with light for 4 hours in a quartz cell (manufactured by Fine, 4 clear windows for spectroscopy) using a 100 W high-pressure mercury lamp (manufactured by USHIO INC., lamp: UM-102, power supply: UM-103B-B). After completion of the reaction, the solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:9 to 5:5) as the eluent to obtain 42 mg of the desired product as white crystals.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09434684B2uspto-grants-2016_09