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Potassium Carbonate → HCID 178434289、化合物

HRID 1880394
ノート
印刷プレビュー

反応式

HRID 1880394 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

HCID 178434289HCID 178434289、化合物収率 80.3%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 22242641Methanol--water (1/1)溶媒

実験手順

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%).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-c013c2b41cb644f7bd25d2831c79fc2e
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08318762B2

反応ノート

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