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

HRID 650007노트

반응식

HRID 650007 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-a4db94400f894aad879fe15e4a33e021
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06271225B1

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