Methane, dichloromethoxy- → 2-Formylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one

HRID 650005노트

반응식

HRID 650005 반응식
[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.Cl[CH:17]([O:19]C)Cl.[Cl-].[Al+3].[Cl-].[Cl-]>C(Cl)Cl>[CH:17]([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]

참가 물질

5

반응물 3

HCID 21004Methane, dichloromethoxy-HCID 6451240Aluminum(III) ChlorideHCID 18422172Thieno[2,3-b][1,5]benzoxazepin-4(5H)-one

생성물 1

HCID 184221402-Formylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one수율 55.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Thieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.9 g) was suspended in methylene chloride (20 ml) and dichloromethylmethyl ether (4.0 g) was added. To this reaction system was added aluminum chloride (4.6 g) under ice-cooling and the mixture was stirred for 15 minutes. The reaction mixture was poured into ice water-chloroform and the mixture was stirred at room temperature for 20 minutes. The aqueous layer was extracted 5 times with chloroform and the combined organic layer was dried over sodium sulfate. The solvent was evaporated under reduced pressure and diisopropyl ether was added to the residue. The precipitated crystals were collected by filtration to give 2-formylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.2 g).

후처리

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 20 minutes
  3. extractionThe aqueous layer was extracted 5 times with chloroform
  4. dry with materialthe combined organic layer was dried over sodium sulfate
  5. customThe solvent was evaporated under reduced pressure and diisopropyl ether
  6. additionwas added to the residue
  7. filtrationThe precipitated crystals were collected by filtration

출처 및 근거

ORD 기록
ord-6dbfef6b15ff49c0a27ad94d5e9a03dc
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06271225B1

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