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Methane → 5-[2,6-Dichloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoyl chloride

HRID 1902997
ノート
印刷プレビュー

反応式

HRID 1902997 の反応式
[Cl:1][C:2]1[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[C:17]([Cl:25])[C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:14]([O-:16])=[O:15])=[C:9]([CH:13]=1)[C:10]([OH:12])=O.CN(C)C=O.S(Cl)([Cl:33])=O.C>ClCCCl>[Cl:1][C:2]1[CH:20]=[C:19]([C:21]([F:24])([F:22])[F:23])[CH:18]=[C:17]([Cl:25])[C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:14]([O-:16])=[O:15])=[C:9]([CH:13]=1)[C:10]([Cl:33])=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 297MethaneHCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 13013695HCID 13013695、化合物

生成物 1

HCID 129267235-[2,6-Dichloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoyl chloride収率 79%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane
溶媒

実験手順

79.2 g of 5-(2,6-dichloro-4-trifluoromethyl-phenoxy)-2-nitro-benzoic acid and 0.5 ml of dimethylformamide were introduced into 150 ml of 1,2-dichloro-ethane. 28.6 g of thionyl chloride were added dropwise at 60° to 65° C. and the mixture was heated under reflux for 1 hour. The solution was clarified with active charcoal and filtered through kieselguhr. The mother liquor was concentrated and the residue was recrystallized from cyclohexane. 65.1 g (79% of theory) of 5-(2,6-dichloro-4-trifluoromethyl-phenoxy)-2-nitro-benzoic acid chloride, of melting point 95° C., were obtained.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1 hour
  3. filtrationfiltered through kieselguhr
  4. concentrationThe mother liquor was concentrated
  5. customthe residue was recrystallized from cyclohexane

出典と根拠

ORDレコード
ord-e5f96fcfec41459dbfa537cd76b2d1dc
出典データセット
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04435208

反応ノート

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