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Benzophenone → N-[(2Z)-2-[3-chloro-5-(trifluoromethyl)-2-pyridinyl]-2-ethoxyiminoethyl]-2-(trifluoromethyl)benzamide

HRID 56004
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HRID 56004 반응식
[Cl:1][C:2]1[C:3]([C:12](=[N:27][O:28][CH2:29][CH3:30])[CH2:13][NH:14][C:15](=[O:26])[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22]([F:25])([F:24])[F:23])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.C(C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(#N)C>[Cl:1][C:2]1[C:3](/[C:12](=[N:27]\[O:28][CH2:29][CH3:30])/[CH2:13][NH:14][C:15](=[O:26])[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22]([F:24])([F:25])[F:23])=[N:4][CH:5]=[C:6]([C:8]([F:9])([F:11])[F:10])[CH:7]=1
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참가 물질

4

반응물 2

HCID 3102BenzophenoneHCID 131736890HCID 131736890, 화합물

생성물 1

HCID 118071504N-[(2Z)-2-[3-chloro-5-(trifluoromethyl)-2-pyridinyl]-2-ethoxyiminoethyl]-2-(trifluoromethyl)benzamide수율 87.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2f427f502f364bb1a8fb17ec4914a72e
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09434684B2

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