Triethylsilane → 2-propylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one

HRID 650007ノート

反応式

HRID 650007 の反応式
[C:1]([C:5]1[S:19][C:8]2[O:9][C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[NH:12][C:13](=[O:14])[C:7]=2[CH:6]=1)(=O)[CH2:2][CH3:3].C([SiH](CC)CC)C>>[CH2:1]([C:5]1[S:19][C:8]2[O:9][C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[NH:12][C:13](=[O:14])[C:7]=2[CH:6]=1)[CH2:2][CH3:3]

参加物

3

反応物 2

HCID 12052TriethylsilaneHCID 184222072-propionylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one

生成物 1

HCID 184223102-propylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one収率 81.7%

実験手順

2-Propionylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.2 g) was dissolved in trifuoroacetic acid (20 ml) and triethylsilane (2 g) was added. The mixture was stirred at room temperature for 20 hours. The solvent was evaporated under reduced pressure and the residue was dissolved in chloroform. The mixture was washed with water and saturated aqueous sodium hydrogencarbonate solution and dried over sodium sulfate. The solvent was evaporated under reduced pressure. To the residue were added chloroform and ethyl acetate and the precipitated crystals were collected by filtration. The obtained crystals were washed with diisopropyl ether to give 2-propylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (930 mg).

後処理

  1. additionwas added
  2. customThe solvent was evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in chloroform
  4. washThe mixture was washed with water and saturated aqueous sodium hydrogencarbonate solution
  5. dry with materialdried over sodium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. additionTo the residue were added chloroform and ethyl acetate
  8. filtrationthe precipitated crystals were collected by filtration
  9. washThe obtained crystals were washed with diisopropyl ether

出典と根拠

ORDレコード
ord-a4db94400f894aad879fe15e4a33e021
出典データセット
uspto-grants-2001_08
特許番号
US06271225B1

反応ノート

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