Trifluoroacetic acid → HCID 68616622、化合物

HRID 1620060ノート

反応式

HRID 1620060 の反応式
C(O)(C(F)(F)F)=O.C(OC(=O)[NH:14][C:15]1[CH:16]=[N:17][CH:18]=[C:19]([C:21]2[O:22][C:23]([CH3:26])=[CH:24][CH:25]=2)[CH:20]=1)(C)(C)C>C(Cl)(Cl)Cl>[CH3:26][C:23]1[O:22][C:21]([C:19]2[CH:20]=[C:15]([NH2:14])[CH:16]=[N:17][CH:18]=2)=[CH:25][CH:24]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 89546857HCID 89546857、化合物

生成物 1

HCID 68616622HCID 68616622、化合物収率 118.7%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

TFA (1 ml) was added to a chloroform solution (2 ml) containing tert-butyl(5-(5-methylfuran-2-yl)pyridin-3-yl)carbamate (61 mg) obtained in the 1st step, stirring at room temperature for 2 hours. The solvent was distilled away under reduced pressure, the obtained residue was dissolved in chloroform, and the resultant was washed with water and a saturated aqueous sodium hydrogen carbonate solution. Subsequently, the aqueous layers were combined, followed by extraction with chloroform (×2). The organic layers was combined and dried over anhydrous sodium sulfate. The solvent was distilled away from the obtained organic layers under reduced pressure, and a white solid of 5-(5-methylfuran-2-yl)pyridin-3-amine (46 mg) was thus obtained.

後処理

  1. customobtained in the 1st step
  2. distillationThe solvent was distilled away under reduced pressure
  3. dissolutionthe obtained residue was dissolved in chloroform
  4. washthe resultant was washed with water
  5. extractionfollowed by extraction with chloroform (×2)
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled away from the obtained organic layers under reduced pressure

出典と根拠

ORDレコード
ord-c57bd9764d5340459d7bed388b3cc92d
出典データセット
uspto-grants-2014_07
特許番号
US08772320B2

反応ノート

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