Bromine → 1-Bromo-3-chloro-2,4-difluoro-5-nitrobenzene

HRID 1165408ノート

反応式

HRID 1165408 の反応式
[F:1][C:2]1[C:7]([Cl:8])=[C:6]([F:9])[CH:5]=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11].[Br:13]Br>ClCCl>[F:1][C:2]1[C:7]([Cl:8])=[C:6]([F:9])[C:5]([Br:13])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11]

参加物

4

反応物 2

HCID 24408BromineHCID 2230803-Chloro-2,4-difluoronitrobenzene

生成物 1

HCID 198616351-Bromo-3-chloro-2,4-difluoro-5-nitrobenzene

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

19.2 g of 2,4-difluoro-3-chloronitrobenzene and 3 g of anhydrous FeCl3 are heated to +140° C., 5.1 ml of bromine are added dropwise with stirring, and the mixture is stirred for a further 48 hours at that temperature. The reaction mixture is cooled and is then taken up in dichloromethane and washed with water. The organic phase is separated off, dried over sodium sulfate and concentrated. The residue is purified on a silica gel column using hexane/dichloromethane (10:1) as eluant. The title compound of formula ##STR10## is obtained in the form of a brown oil; refractive index nD25 : 1.5720.

後処理

  1. stirringthe mixture is stirred for a further 48 hours at that temperature
  2. temperatureThe reaction mixture is cooled
  3. washwashed with water
  4. customThe organic phase is separated off
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue is purified on a silica gel column

出典と根拠

ORDレコード
ord-05ceee95f2ef43088c6b2f4ee654310f
出典データセット
uspto-grants-1990_03
特許番号
US04910018

反応ノート

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