2,4-Dichlorotoluene → 2-Bromo-4,6-dichlorotoluene

HRID 648988

반응식

HRID 648988 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([CH3:9])=[CH:4][CH:3]=1.[Br:10]Br>C(Cl)(Cl)(Cl)Cl.C(Cl)Cl>[Br:10][C:4]1[CH:3]=[C:2]([Cl:1])[CH:7]=[C:6]([Cl:8])[C:5]=1[CH3:9]

참가 물질

5

반응물 2

HCID 72542,4-DichlorotolueneHCID 24408Bromine3회

생성물 1

HCID 102636612-Bromo-4,6-dichlorotoluene수율 213.1%

시약·촉매·용매 2

HCID 5943Carbon Tetrachloride용매HCID 6344Dichloromethane용매

실험 절차

To a mixture of 32 g of 4,6-dichlorotoluene and 0.3 g of anhydrous FeCl3, add, with stirring, 10 g of bromine in 1 g portions while maintaining a temperature of 20°-25° C. Add thereto a solution of 22 g of bromine in 100 mL of CCl4 slowly while maintaining a temperature of 20°-25° C. After the addition of bromine is complete, stir the mixture so formed for 15 min, and dilute the reaction mixture with 200 mL of CH2Cl2, and wash the organic solution with 5% aqueous sodium thiosulfate. Dry the organic layer over anhydrous K2CO3, filter, and evaporate to a residue. Recrystallize the residue from CH3CN to give 32 g of 2-bromo-4,6-dichlorotoluene, mp 84°-5° C.

후처리

  1. additionadd
  2. additionAdd
  3. stirringstir the mixture
  4. customso formed for 15 min
  5. washwash the organic solution with 5% aqueous sodium thiosulfate
  6. dry with materialDry the organic layer over anhydrous K2CO3
  7. filtrationfilter
  8. customevaporate to a residue
  9. customRecrystallize the residue from CH3CN

출처 및 근거

ORD 기록
ord-438b09bd1d5145b0b8c540d001993b3c
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04737508

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