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

HRID 1281878ノート

反応式

HRID 1281878 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:19])[CH2:17][CH3:18].[Cl-].[Al+3].[Cl-].[Cl-]>ClCCCl>[C: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)(=[O:19])[CH2:17][CH3:18]

参加物

5

反応物 3

HCID 62324Propionyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 18422172Thieno[2,3-b][1,5]benzoxazepin-4(5H)-one

生成物 1

HCID 184222072-propionylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one収率 74.2%

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 propionyl chloride (770 mg) was added. To this reaction system was added portionwise aluminum chloride (4.7 g) under ice-cooling. Insoluble matter was filtrated, and the filtrate was poured into ice water and chloroform was added. The aqueous layer was extracted twice with chloroform and the combined organic layer was dried over sodium sulfate. The solvent was evaporated under reduced pressure and the precipitated crystals were collected by filtration to give 2-propionylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.4 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. extractionThe aqueous layer was extracted twice with chloroform
  6. dry with materialthe combined organic layer was dried over sodium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. filtrationthe precipitated crystals were collected by filtration

出典と根拠

ORDレコード
ord-fe6efc1e841c472aab1ae5c9bf8f747b
出典データセット
uspto-grants-2002_09
特許番号
US06455521B1

反応ノート

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