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Potassium Carbonate → 2-(4-Chloro-5-fluoro-2-formyl-phenoxy)-2-methyl-propionic acid methyl ester

HRID 658944
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인쇄 미리보기

반응식

HRID 658944 반응식
[Cl:1][C:2]1[C:3]([F:11])=[CH:4][C:5]([OH:10])=[C:6]([CH:9]=1)[CH:7]=[O:8].[CH3:12][O:13][C:14](=[O:19])[C:15](Br)([CH3:17])[CH3:16].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:12][O:13][C:14](=[O:19])[C:15]([O:10][C:5]1[CH:4]=[C:3]([F:11])[C:2]([Cl:1])=[CH:9][C:6]=1[CH:7]=[O:8])([CH3:17])[CH3:16]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 90097Methyl 2-bromo-2-methylpropionateHCID 71721325-Chloro-4-fluoro-2-hydroxybenzaldehyde

생성물 1

HCID 595493062-(4-Chloro-5-fluoro-2-formyl-phenoxy)-2-methyl-propionic acid methyl ester수율 85.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
140 °C

실험 절차

A mixture of 5-chloro-4-fluoro-2-hydroxy-benzaldehyde (0.8 g, 4.6 mmol), 2-bromo-2-methyl-propionic acid methyl ester (1.6 g, 9.2 mmol) and K2CO3 (2 g, 14.5 mmol) in DMF (40 mL) was placed in a sealed tube and heated by irradiation in microwave reactor at 140° C. for 12 min. After cooled to room temperature, the mixture was partitioned between EtOAc and water. The organic layer was separated, washed with water, dried over anhydrous Na2SO4 and concentrated to give the thitle compound as a brown solid (1.08 g).

후처리

  1. customwas placed in a sealed tube
  2. temperatureAfter cooled to room temperature
  3. customthe mixture was partitioned between EtOAc and water
  4. customThe organic layer was separated
  5. washwashed with water
  6. dry with materialdried over anhydrous Na2SO4
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5ebe632a002149bdbfb6092a30ca81ee
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08076482B2

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