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

HRID 1165408노트

반응식

HRID 1165408 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-05ceee95f2ef43088c6b2f4ee654310f
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04910018

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