Butyryl chloride → 2-butylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one

HRID 650004ノート

反応式

HRID 650004 の反応式
[S:1]1[C:5]2[O:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[NH:9][C:10](=[O:11])[C:4]=2[CH:3]=[CH:2]1.[C:16](Cl)(=O)[CH2:17][CH2:18][CH3:19].[Cl-].[Al+3].[Cl-].[Cl-]>ClCCCl>[CH2:16]([C:2]1[S:1][C:5]2[O:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[NH:9][C:10](=[O:11])[C:4]=2[CH:3]=1)[CH2:17][CH2:18][CH3:19]

参加物

5

反応物 3

HCID 8855Butyryl chlorideHCID 6451240Aluminum(III) ChlorideHCID 18422172Thieno[2,3-b][1,5]benzoxazepin-4(5H)-one

生成物 1

HCID 184222972-butylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one収率 63.6%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

Thieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.5 g) was suspended in 1,2-dichloroethane (20 ml) and butyryl chloride (880 mg) was added. To this reaction system was added portionwise aluminium chloride (4.6 g) under ice-cooling. The mixture was stirred at room temperature for 45 minutes. Insoluble matter was filtrated and the filtrate was poured into ice water, and chloroform was added. The organic layer was washed with water and dried over sodium sulfate. The solvent was evaporated under reduced pressure and water-ethanol was added. The precipitated crystals were collected by filtration. The obtained crystals were washed with chloroform-diisopropyl ether to give 2-butylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.2 g).

後処理

  1. temperaturecooling
  2. filtrationInsoluble matter was filtrated
  3. additionthe filtrate was poured into ice water, and chloroform
  4. additionwas added
  5. washThe organic layer was washed with water
  6. dry with materialdried over sodium sulfate
  7. customThe solvent was evaporated under reduced pressure and water-ethanol
  8. additionwas added
  9. filtrationThe precipitated crystals were collected by filtration
  10. washThe obtained crystals were washed with chloroform-diisopropyl ether

出典と根拠

ORDレコード
ord-d9a696ea63cf4e42b81a65cdd85aa3ef
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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