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

HRID 1281882노트

반응식

HRID 1281882 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>FC(F)(F)C(O)=O>[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

4

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%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

2-Propionylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.2 g) was dissolved in trifluoroacetic 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. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in chloroform
  3. washThe mixture was washed with water and saturated aqueous sodium hydrogencarbonate solution
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. additionTo the residue were added chloroform and ethyl acetate
  7. filtrationthe precipitated crystals were collected by filtration
  8. washThe obtained crystals were washed with diisopropyl ether

출처 및 근거

ORD 기록
ord-fafd55ddda5744d8b49babc0196f1011
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06455521B1

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