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

HRID 1871865

反応式

HRID 1871865 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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. This solution was cooled to 0° C., to which 75 g of the crude crystals of 2-fluoro-4-chloro-5-hydroxyphenylhydrazine hydrochloride was added. The mixture was stirred at room temperature for 70 minutes, and the resulting 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).

後処理

  1. temperaturethe solution was heated at 80° to 90° C. for 40 minutes
  2. additionwas added
  3. filtrationthe resulting crystals were collected by filtration
  4. customdried under reduced pressure, which

出典と根拠

ORDレコード
ord-0f23a5c7a3574afda4a3bdeea1036847
出典データセット
uspto-grants-2000_08
特許番号
US06107250

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