N-[2-(3,5-dichloropyridin-2-yl)-2-(ethoxyimino)ethyl]-2-(trifluoromethyl)benzamide → N-[(2Z)-2-(3,5-dichloro-2-pyridinyl)-2-ethoxyiminoethyl]-2-(trifluoromethyl)benzamide

HRID 55981ノート

反応式

HRID 55981 の反応式
[Cl:1][C:2]1[C:3]([C:9](=[N:24][O:25][CH2:26][CH3:27])[CH2:10][NH:11][C:12](=[O:23])[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[C:19]([F:22])([F:21])[F:20])=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1>C(#N)C>[Cl:1][C:2]1[C:3](/[C:9](=[N:24]\[O:25][CH2:26][CH3:27])/[CH2:10][NH:11][C:12](=[O:23])[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[C:19]([F:21])([F:20])[F:22])=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1

参加物

3

反応物 1

HCID 131736883N-[2-(3,5-dichloropyridin-2-yl)-2-(ethoxyimino)ethyl]-2-(trifluoromethyl)benzamide

生成物 1

HCID 118071503N-[(2Z)-2-(3,5-dichloro-2-pyridinyl)-2-ethoxyiminoethyl]-2-(trifluoromethyl)benzamide収率 21.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

190 mg of N-[2-(3,5-dichloropyridin-2-yl)-2-(ethoxyimino)ethyl]-2-(trifluoromethyl)benzamide was dissolved in 4 ml of acetonitrile, and the solution was irradiated with light for 2.5 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 3:7) as the eluent to obtain 41.3 mg of the desired product as white crystals.

後処理

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

出典と根拠

ORDレコード
ord-14fcdf7ccf6e4475804e6698de7f0131
出典データセット
uspto-grants-2016_09
特許番号
US09434684B2

反応ノート

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