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Hydrochloric Acid → 4-Bromo-alpha-chloro-3-methylbenzaldoxime

HRID 878801
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HRID 878801 반응식
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([CH:6]=[N:7][OH:8])=[CH:4][C:3]=1[CH3:11].[ClH:12].Cl[O-].[Na+]>O1CCCC1>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([Cl:12])=[N:7][OH:8])=[CH:4][C:3]=1[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 23665760Sodium HypochloriteHCID 738479544-Bromo-3-methylbenzaldehyde oxime

생성물 1

HCID 866114784-Bromo-alpha-chloro-3-methylbenzaldoxime수율 98.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In a solution of 82.0 g of 4-bromo-3-methylbenzaldoxime in 450 mL of tetrahydrofuran, 120.0 g of concentrated hydrochloric acid was added dropwise under cooling with ice and with stirring over 45 minutes. Then, 220 mL of 8% sodium hypochlorite aqueous solution was added dropwise over 75 minutes carefully so that the temperature of the reaction mixture would not exceed 5° C. After the completion of the addition dropwise, it was continued to stir at a temperature of 10° C. or less for further 90 minutes. After the completion of the reaction, the reaction mixture was blown with nitrogen gas for 45 minutes, then precipitated insoluble material was filtered off, tetrahydrofuran was distilled off under reduced pressure. The residual aqueous solution was extracted with 240.0 g of ethyl acetate, and the organic phase was washed with water (240 mL×2). The insoluble material was filtered off, the solvent was distilled off under reduced pressure to obtain 93.5 g of the aimed product as pale yellow crystal.

후처리

  1. temperatureunder cooling with ice
  2. customexceed 5° C
  3. additionAfter the completion of the addition dropwise
  4. stirringto stir at a temperature of 10° C. or less for further 90 minutes
  5. customAfter the completion of the reaction
  6. waitthe reaction mixture was blown with nitrogen gas for 45 minutes
  7. filtrationprecipitated insoluble material was filtered off
  8. distillationtetrahydrofuran was distilled off under reduced pressure
  9. extractionThe residual aqueous solution was extracted with 240.0 g of ethyl acetate
  10. washthe organic phase was washed with water (240 mL×2)
  11. filtrationThe insoluble material was filtered off
  12. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-414f076d7ec14d0ea1f19436139cc557
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08987464B2

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