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Trifluoroacetic acid → HCID 136388334、化合物

HRID 1861905
ノート
印刷プレビュー

反応式

HRID 1861905 の反応式
C(OC(=O)[NH:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([NH:15][C:16]([NH2:21])=[N:17][N+:18]([O-:20])=[O:19])[CH:10]=1)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[N+:18]([N:17]=[C:16]([NH2:21])[NH:15][C:11]1[CH:10]=[C:9]([CH2:8][NH2:7])[CH:14]=[CH:13][CH:12]=1)([O-:20])=[O:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 136388335HCID 136388335、化合物

生成物 1

HCID 136388334HCID 136388334、化合物収率 75.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of the compound (230 mg) obtained in Example 33, methylene chloride (3 ml) and trifluoroacetic acid (1.15 ml) was stirred at room temperature for 3 h. The reaction mixture was concentrated under reduced pressure and 25% aqueous ammonia solution was added to the resulting residue, and the reaction mixture was extracted with chloroform. The organic layer was washed with a saturated aqueous sodium chloride solution and dried with anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent; methanol) to give 117 mg of the titled compound (yield, 75%).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure and 25% aqueous ammonia solution
  2. additionwas added to the resulting residue
  3. extractionthe reaction mixture was extracted with chloroform
  4. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  5. dry with materialdried with anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent; methanol)

出典と根拠

ORDレコード
ord-50674ecde2664803a2aa2703fd0eddbb
出典データセット
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06534546B1

反応ノート

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