Sodium Hydroxide → 4-Bromo-3,5-diethoxybenzoic acid

HRID 38480ノート

反応式

HRID 38480 の反応式
[Br:1][C:2]1[C:11]([O:12][CH2:13][CH3:14])=[CH:10][C:5]([C:6]([O:8]C)=[O:7])=[CH:4][C:3]=1[O:15][CH2:16][CH3:17].[OH-].[Na+]>C1COCC1.CO>[Br:1][C:2]1[C:11]([O:12][CH2:13][CH3:14])=[CH:10][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[O:15][CH2:16][CH3:17]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 57930905Methyl 4-bromo-3,5-diethoxybenzoate

生成物 1

HCID 579309874-Bromo-3,5-diethoxybenzoic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of methyl 4-bromo-3,5-diethoxybenzoate (3.00 g) in a mixture of THF (25 ml) and MeOH (10 ml) was added aqueous 1N NaOH (20 ml) and the reaction mixture was stirred at room temperature for 6 h. The mixture was concentrated under reduced pressure and the residue was diluted with H2O and diethylether. The aqueous layer was acidified with aqueous 1N HCl, the mixture was extracted with CHCl3 and dried over sodium sulfate. After filtration and concentration, the residue was dried in vacuo to give the crude intended compound as a colorless solid. Thus obtained crude product was used in the next step without further purification.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additionthe residue was diluted with H2O and diethylether
  3. extractionthe mixture was extracted with CHCl3
  4. dry with materialdried over sodium sulfate
  5. filtrationAfter filtration and concentration
  6. customthe residue was dried in vacuo
  7. customto give the crude
  8. customThus obtained crude product
  9. customwas used in the next step without further purification

出典と根拠

ORDレコード
ord-a47a94cc5a9e4777ab1d821f29080afe
出典データセット
uspto-grants-2013_09
特許番号
US08524730B2

反応ノート

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