Water → 2,6-Bis-benzyloxybenzoic Acid Benzyl Ester

HRID 660617

反応式

HRID 660617 の反応式
O[C:2]1[CH:10]=[CH:9][CH:8]=[C:7](O)[C:3]=1[C:4](O)=[O:5].[CH2:12](Br)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[C:20]([O-:23])([O-])=[O:21].[K+].[K+].[OH2:26]>CN(C=O)C>[CH2:12]([O:23][C:20](=[O:21])[C:2]1[C:10]([O:26][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:9][CH:8]=[CH:7][C:3]=1[O:5][CH2:4][C:3]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:2]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

6

反応物 4

HCID 962WaterHCID 7498Benzyl BromideHCID 93382,6-Dihydroxybenzoic AcidHCID 11430Potassium Carbonate

生成物 1

HCID 145620262,6-Bis-benzyloxybenzoic Acid Benzyl Ester

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2,6-dihydroxybenzoic acid (1.54 g, 10 mmol) and benzyl bromide (3.63 mL, 30.5 mmol) in DMF (20 mL) is added K2CO3 (4.83 g, 30.5 mmol) and the mixture is stirred at RT for 48 h. Water is added and the mixture is extracted with EtOAc. The organic phase is washed with water and brine then is dried over sodium sulfate. The solvent is removed under reduced pressure and the residue is purified by flash chromatography using hexane/EtOAc (8:1) as eluent to give the title compound.

後処理

  1. extractionthe mixture is extracted with EtOAc
  2. washThe organic phase is washed with water and brine
  3. dry with materialthen is dried over sodium sulfate
  4. customThe solvent is removed under reduced pressure
  5. customthe residue is purified by flash chromatography

出典と根拠

ORDレコード
ord-a81e8126fd804bb4b76982e317e953de
出典データセット
uspto-grants-2011_12
特許番号
US08084448B2

関連ノート

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