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

HRID 1089169

反応式

HRID 1089169 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 147486362,3-Dichloro-4,5-dihydroxybenzaldehyde収率 91.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f431b2249bc24617958698cdfade4a67
出典データセット
uspto-grants-1990_10
特許番号
US04965282

関連ノート

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