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Chlorine → HCID 74003410、化合物

HRID 1489389
ノート
印刷プレビュー

反応式

HRID 1489389 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24526ChlorineHCID 807690HCID 807690、化合物

生成物 1

HCID 74003410HCID 74003410、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dda38af0a33b4138b9d56dd55f317ad6
出典データセット
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05677465

反応ノート

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