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

HRID 1281878노트

반응식

HRID 1281878 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.[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-fe6efc1e841c472aab1ae5c9bf8f747b
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06455521B1

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