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Chlorine → HCID 74003410, 화합물

HRID 128910
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HRID 128910 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([CH2:6][O:7][C:8]2[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=2[CH:10]=[N:11][OH:12])=[CH:4][CH:3]=1.[Cl:19]Cl>CCOCC.C(Cl)Cl>[Cl:19][C:10](=[N:11][OH:12])[C:9]1[CH:13]=[CH:14][CH:15]=[CH:16][C:8]=1[O:7][CH2:6][C:5]1[CH:17]=[CH:18][C:2]([Cl:1])=[CH:3][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24526ChlorineHCID 807690HCID 807690, 화합물

생성물 1

HCID 74003410HCID 74003410, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

2-(4-Chlorobenzyloxy)benzaldehyde oxime (26.17 g) was dissolved in ether (200 ml) and methylene chloride (50 ml), and chlorine (6.0 ml) was introduced at -10° C. or below, and then the temperature was raised from -10° C. to room temperature over 2 hours. After completion of the reaction, the mixture was concentrated under reduced pressure to give crude α-chloro-2-(4-chlorobenzyloxy)benzaldehyde oxime. The resulting crude product was dissolved in acetonitrile (150 ml), a mixture of imidazole (17.02 g) and acetonitrile (100 ml) was added at room temperature over 15 minutes, and then the resulting mixture was stirred at 65 to 70° C. for 2 hours. After completion of the reaction, water and methylene chloride were added. The resulting crystals were separated by filtration to give 2-(4-chlorobenzyloxy)-α-(1-imidazolyl)benzaldehyde oxime (11.05 g) as colorless crystals. mp. 196°-197° C.

후처리

  1. temperaturethe temperature was raised from -10° C. to room temperature over 2 hours
  2. customAfter completion of the reaction
  3. concentrationthe mixture was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3b784ba25295427ebd97aea3280fb055
출처 데이터셋
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05466661

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