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Potassium Carbonate → 5-Methylsulfonyl-2-(2,2,2-trifluoro-1-methylethoxy)benzoic acid methyl ester

HRID 1930975
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인쇄 미리보기

반응식

HRID 1930975 반응식
[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[C:8]([S:10]([CH3:13])(=[O:12])=[O:11])[CH:7]=[CH:6][C:5]=1[OH:14].[F:16][C:17]([F:29])([F:28])[CH:18](OS(C(F)(F)F)(=O)=O)[CH3:19].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[C:8]([S:10]([CH3:13])(=[O:12])=[O:11])[CH:7]=[CH:6][C:5]=1[O:14][CH:18]([CH3:19])[C:17]([F:29])([F:28])[F:16]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 235031632-Hydroxy-5-methylsulfonylbenzoic acid methyl esterHCID 574452801, 1, 1-Trifluoropropan-2-yl trifluoromethanesulfonatc

생성물 1

HCID 588633505-Methylsulfonyl-2-(2,2,2-trifluoro-1-methylethoxy)benzoic acid methyl ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A mixture of 21.7 mmol 2-hydroxy-5-methanesulfonyl-benzoic acid methyl ester (WO 2002074774), 32.5 mmol trifluoro-methanesulfonic acid 2,2,2-trifluoro-1-methyl-ethyl ester [212556-43-9] and 43.4 mmol potassium carbonate in 87 ml DMF was stirred at 80° C. for 48 hours. After cooling to room temperature, the mixture was concentrated in vacuo, resuspended in water and stirred for 1 hour. Filtration yielded the title compound.

후처리

  1. temperatureAfter cooling to room temperature
  2. concentrationthe mixture was concentrated in vacuo
  3. stirringstirred for 1 hour
  4. filtrationFiltration

출처 및 근거

ORD 기록
ord-21b4dbe934e64af1932f6c63b9b863b4
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08188139B2

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