Water → 3,3,3-Trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone)

HRID 1018426

반응식

HRID 1018426 반응식
C([O-])(=O)C.[Na+].O.Br[CH:8](Br)[C:9]([C:11]([F:14])([F:13])[F:12])=[O:10].[F:16][C:17]1[CH:22]=[C:21]([Cl:23])[C:20]([O:24][CH:25]([CH3:27])[CH3:26])=[CH:19][C:18]=1[NH:28][NH2:29]>C(OCC)C>[Cl:23][C:21]1[C:20]([O:24][CH:25]([CH3:26])[CH3:27])=[CH:19][C:18]([NH:28][N:29]=[CH:8][C:9](=[O:10])[C:11]([F:14])([F:13])[F:12])=[C:17]([F:16])[CH:22]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 185080(4-Chloro-2-fluoro-5-propan-2-yloxyphenyl)hydrazineHCID 517045Sodium AcetateHCID 5505231,1-Dibromo-3,3,3-trifluoroacetone

생성물 1

HCID 691414303,3,3-Trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone)

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a mixed solution of 5.3 g (53.5 mmol) of sodium acetate and about 100 ml of water was added under ice cooling 6.6 g (24.3 mmol) of 1,1-dibromo-3,3,3-trifluoroacetone, and the reaction was allowed to proceed at 70° C. for 20 minutes. Then, the reaction mixture was cooled to room temperature, to which a solution of 5.8 g (21.5 mmol) of 2-fluoro-4-chloro-5-isopropoxyphenylhydrazine dissolved in about 20 ml of diethyl ether was added, and the reaction mixture was stirred at room temperature for 1 hour. The ether layer was separated, washed once with 10 ml of saturated sodium chloride solution, and dried with magnesium sulfate. The diethyl ether was distilled out, which afforded 6.5 g (20.0 mmol) of 3,3,3-trifluoro-2-oxo-propanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone).

후처리

  1. additionwas added
  2. customThe ether layer was separated
  3. washwashed once with 10 ml of saturated sodium chloride solution
  4. dry with materialdried with magnesium sulfate
  5. distillationThe diethyl ether was distilled out

출처 및 근거

ORD 기록
ord-2317561dc763454e9eda6a44825922c9
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06482773B1

연결된 노트

불러오는 중…