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Potassium Carbonate → HCID 178434289, 화합물

HRID 1880394
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HRID 1880394 반응식
[CH3:1][C:2]1[C:10]2[C:5](=[CH:6][C:7](C(OC)=O)=[CH:8][CH:9]=2)[N:4](S(C(F)(F)F)(=O)=O)[N:3]=1.[C:22]([O-])([O-:24])=[O:23].[K+].[K+]>CO.O.CCOC(C)=O>[CH3:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:22]([OH:24])=[O:23])[CH:9]=2)[NH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 22663352Methyl 1-triflyl-3-methyl-indazole-6-carboxylate

생성물 1

HCID 178434289HCID 178434289, 화합물수율 80.3%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 22242641Methanol--water (1/1)용매

실험 절차

To a solution of methyl 3-methyl-1-[(trifluoromethyl)sulfonyl]-1H-indazole-6-carboxylate (590 mg, 1.83 mmol) in methanol/water (3:1, 72 mL) was added K2CO3 (1.01 g, 7.31 mmol) and the mixture was heated at reflux for 2 hours. The reaction was cooled to room temperature and the methanol was removed under reduced pressure. The aqueous solution was acidified to pH 3-3.5 with KHSO4. The solid was isolated by filtration, dissolved in EtOAc and washed with water. The organic layer was dried over Na2SO4, filtered and concentrated to provide the title compound (259 mg, 80%).

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후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. customthe methanol was removed under reduced pressure
  4. customThe solid was isolated by filtration
  5. washwashed with water
  6. dry with materialThe organic layer was dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c013c2b41cb644f7bd25d2831c79fc2e
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318762B2

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