Potassium Carbonate → (2-Acetyl-3-hydroxy-phenoxy)-acetic acid tert-butyl ester

HRID 29478

反応式

HRID 29478 の反応式
[CH3:1][C:2]([C:4]1[C:5]([OH:11])=[CH:6][CH:7]=[CH:8][C:9]=1[OH:10])=[O:3].C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21]>CC(C)=O>[C:23]([O:22][C:20](=[O:21])[CH2:19][O:11][C:5]1[CH:6]=[CH:7][CH:8]=[C:9]([OH:10])[C:4]=1[C:2](=[O:3])[CH3:1])([CH3:26])([CH3:25])[CH3:24]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 696872',6'-DihydroxyacetophenoneHCID 79177tert-Butyl bromoacetate

生成物 1

HCID 68714827(2-Acetyl-3-hydroxy-phenoxy)-acetic acid tert-butyl ester

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A solution of 2,6-dihydroxyacetophenone (35.37 g, 0.23 moles), potassium carbonate (51.4 g, 0.37 moles), and t-butyl bromoacetate (28.4 mL, 0.23 moles) in 440 mL of acetone was heated at reflux for 1.5 hours. It was then cooled to room temperature and filtered. The filter cake was washed with acetone and the combined mother liquors were concentrated in vacuo. (2-Acetyl-3-hydroxy-phenoxy)-acetic acid tert-butyl ester was isolated as thick yellow oil, which was used directly used for the next step.

後処理

  1. temperatureat reflux for 1.5 hours
  2. filtrationfiltered
  3. washThe filter cake was washed with acetone
  4. concentrationthe combined mother liquors were concentrated in vacuo

出典と根拠

ORDレコード
ord-110f91f4fca842a19f7388dc5a948ecb
出典データセット
uspto-grants-2008_09
特許番号
US07420001B2

関連ノート

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