Water → 2,3-Dichloro-4,5-dihydroxybenzaldehyde

HRID 1074186

반응식

HRID 1074186 반응식
B(Br)(Br)Br.[Cl:5][C:6]1[C:13]([Cl:14])=[C:12]([O:15]C)[C:11]([O:17]C)=[CH:10][C:7]=1[CH:8]=[O:9].O>C(Cl)Cl>[Cl:5][C:6]1[C:13]([Cl:14])=[C:12]([OH:15])[C:11]([OH:17])=[CH:10][C:7]=1[CH:8]=[O:9]

참가 물질

5

반응물 3

HCID 962WaterHCID 25134Boron tribromideHCID 147486342,3-Dichloro-4,5-dimethoxybenzaldehyde

생성물 1

HCID 147486362,3-Dichloro-4,5-dihydroxybenzaldehyde수율 91.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 2.51 g of boron tribromide in methylene chloride is added to dropwise to a solution of 0.47 g of 2,3-dichloro-4,5-dimethoxybenzaldehyde in methylene chloride at -50° to -60° C. and the mixture is stirred at -50° C. to room temperature for 1 hour. The reaction mixture is poured into water and the aqueous mixture is extracted with ethyl acetate. The extract is evaporated to remove solvent. Methanol and 10% hydrochloric acid are added to the residue and the mixture is stirred at room temperature for 1 hour. To the reaction mixture are added water, and the mixture is extracted with ethyl acetate. The extract is washed with water, dried and evaporated to remove solvent. The residue is washed with n-hexane and dried to give 0.38 g of 2,3-dichloro-4,5-dihydroxybenzaldehyde.

후처리

  1. extractionthe aqueous mixture is extracted with ethyl acetate
  2. customThe extract is evaporated
  3. customto remove solvent
  4. additionMethanol and 10% hydrochloric acid are added to the residue
  5. stirringthe mixture is stirred at room temperature for 1 hour
  6. additionTo the reaction mixture are added water
  7. extractionthe mixture is extracted with ethyl acetate
  8. washThe extract is washed with water
  9. customdried
  10. customevaporated
  11. customto remove solvent
  12. washThe residue is washed with n-hexane
  13. customdried

출처 및 근거

ORD 기록
ord-608913d6f05d4ee0ba42ff4c3a38b503
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04973600

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