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Ethyl Acetate → N-(6-(4-chlorophenyl)-1H-indazol-3-yl)butyramide

HRID 497638
ノート
印刷プレビュー

反応式

HRID 497638 の反応式
[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[Cl:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]2[CH:34]=[C:33]3[C:29]([C:30]([NH:43][C:44](=[O:48])[CH2:45][CH2:46][CH3:47])=[N:31][N:32]3COCC[Si](C)(C)C)=[CH:28][CH:27]=2)=[CH:22][CH:21]=1.C(OCC)(=O)C>O1CCCC1>[Cl:19][C:20]1[CH:21]=[CH:22][C:23]([C:26]2[CH:34]=[C:33]3[C:29]([C:30]([NH:43][C:44](=[O:48])[CH2:45][CH2:46][CH3:47])=[N:31][NH:32]3)=[CH:28][CH:27]=2)=[CH:24][CH:25]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 2724141Tetrabutylammonium FluorideHCID 22319489HCID 22319489、化合物

生成物 1

HCID 22319587N-(6-(4-chlorophenyl)-1H-indazol-3-yl)butyramide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
65 °C

実験手順

9.5 cm3 of tetrabutylammonium fluoride as a 1M solution in tetrahydrofuran are added to a solution of 600 mg of N-[6-(4-chlorophenyl)-1-[[2-(trimethylsilyl)ethoxy]-methyl]-1H-indazol-3-yl]butanamide, prepared previously, in 20 cm3 of tetrahydrofuran, the reaction medium is then heated at about 65° C. for 18 hours and the heating is stopped to add 40 cm3 of ethyl acetate. The organic phase is washed with 2×30 cm3 of saturated aqueous sodium hydrogen carbonate solution and then with 30 cm3 of saturated aqueous sodium chloride solution. The organic phase is dried over magnesium sulphate, filtered and evaporated under reduced pressure (2 kPa; 50° C.). After drying (90 Pa; 50° C.), 238 mg of N-[6-(4-chlorophenyl)-1H-indazol-3-yl]butanamide are obtained in the form of a beige-coloured powder.

後処理

  1. washThe organic phase is washed with 2×30 cm3 of saturated aqueous sodium hydrogen carbonate solution
  2. dry with materialThe organic phase is dried over magnesium sulphate
  3. filtrationfiltered
  4. customevaporated under reduced pressure (2 kPa; 50° C.)
  5. dry with materialAfter drying (90 Pa; 50° C.), 238 mg of N-[6-(4-chlorophenyl)-1H-indazol-3-yl]butanamide
  6. customare obtained in the form of a beige-coloured powder

出典と根拠

ORDレコード
ord-63672352fcf84c4381ac2a9805e1c63d
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06949579B2

反応ノート

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