Trifluoroacetic acid → HCID 68616622、化合物

HRID 2406708ノート

反応式

HRID 2406708 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-369de32a9b484d26a754616941e3eec4
出典データセット
uspto-grants-2014_08
特許番号
US08809371B2

反応ノート

読み込み中…