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Potassium Bicarbonate → 3-(4-Bromo-3-methylphenyl)-5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazole

HRID 552618
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HRID 552618 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]([C:11]([F:14])([F:13])[F:12])=[CH2:10])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[Br:15][C:16]1[CH:25]=[CH:24][C:19]([C:20](Cl)=[N:21][OH:22])=[CH:18][C:17]=1[CH3:26].C(=O)([O-])O.[K+]>O1CCCC1>[Br:15][C:16]1[CH:25]=[CH:24][C:19]([C:20]2[CH2:10][C:9]([C:4]3[CH:3]=[C:2]([Cl:1])[CH:7]=[C:6]([Cl:8])[CH:5]=3)([C:11]([F:14])([F:12])[F:13])[O:22][N:21]=2)=[CH:18][C:17]=1[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516893Potassium BicarbonateHCID 231598231,3-Dichloro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzeneHCID 866114784-Bromo-alpha-chloro-3-methylbenzaldoxime

생성물 1

HCID 231598123-(4-Bromo-3-methylphenyl)-5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazole수율 90.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

In a solution of 22.7 g of 3,5-dichloro-1-(1-trifluoromethylethenyl)benzene produced in Step 1 and 26.0 g of 4-bromo-α-chloro-3-methylbenzaldoxime produced in Step 2 in 120 mL of tetrahydrofuran, 15.7 g of potassium hydrogen carbonate was added, and stirred under reflux with heat for 5 hours. After the completion of the reaction, the reaction mixture was left and cooled to room temperature, insoluble material was filtered off, and then the solvent was distilled off under reduced pressure. 150 mL of water was added in the residue, stirred at room temperature for 18 hours, and then precipitated crystal was filtered off, and dried to obtain 38.6 g of the aimed product as white crystal.

후처리

  1. temperatureunder reflux
  2. temperaturewith heat for 5 hours
  3. customAfter the completion of the reaction
  4. waitthe reaction mixture was left
  5. filtrationinsoluble material was filtered off
  6. distillationthe solvent was distilled off under reduced pressure
  7. addition150 mL of water was added in the residue
  8. stirringstirred at room temperature for 18 hours
  9. customprecipitated crystal
  10. filtrationwas filtered off
  11. customdried

출처 및 근거

ORD 기록
ord-1f439cf9297e44a882eeac32a06c2a5f
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07951828B1

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