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

HRID 29478

반응식

HRID 29478 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-110f91f4fca842a19f7388dc5a948ecb
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07420001B2

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