Sodium Acetate → 3,3,3-Trifluoro-2-oxopropanal (4-chloro-2-fluoro-5-hydroxyphenylhydrazone)

HRID 48498

반응식

HRID 48498 반응식
C([O-])(=O)C.[Na+].Br[CH:7](Br)[C:8]([C:10]([F:13])([F:12])[F:11])=[O:9].Cl.[F:16][C:17]1[CH:22]=[C:21]([Cl:23])[C:20]([OH:24])=[CH:19][C:18]=1[NH:25][NH2:26]>O>[Cl:23][C:21]1[C:20]([OH:24])=[CH:19][C:18]([NH:25][N:26]=[CH:7][C:8](=[O:9])[C:10]([F:13])([F:12])[F:11])=[C:17]([F:16])[CH:22]=1

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 5505231,1-Dibromo-3,3,3-trifluoroacetoneHCID 691421062-Fluoro-4-chloro-5-hydroxyphenylhydrazine hydrochloride

생성물 1

HCID 691427153,3,3-Trifluoro-2-oxopropanal (4-chloro-2-fluoro-5-hydroxyphenylhydrazone)수율 82.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Then, 49.2 g of sodium acetate and 40.5 g of 1,1-dibromo-3,3,3-trifluoroacetone were dissolved in 400 ml of water, and the solution was heated at 80° to 90° C. for 40 minutes. The solution was cooled to 0° C., to which 75 g of the crude 2-fluoro-4-chloro-5-hydroxyphenylhydrazine hydrochloride crystals obtained above was added, and the mixture was stirred at room temperature for 70 minutes. The precipitated crystals were collected by filtration and dried under reduced pressure, which afforded 35.4 g of 3,3,3-trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-hydroxyphenylhydrazone).

후처리

  1. temperaturethe solution was heated at 80° to 90° C. for 40 minutes
  2. customobtained
  3. additionabove was added
  4. filtrationThe precipitated crystals were collected by filtration
  5. customdried under reduced pressure, which

출처 및 근거

ORD 기록
ord-f44e1b90f39141189916bd77ce99a78d
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06703503B2

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