Potassium Carbonate → Methyl 2,4-dichloro-(2-hydroxyiminobut-3-en-4-yl)benzoate

HRID 1276136노트

반응식

HRID 1276136 반응식
Cl.[NH2:2][OH:3].C(=O)([O-])[O-].[K+].[K+].[Cl:10][C:11]1[C:20]([CH:21]=[CH:22][C:23](=O)[CH3:24])=[C:19]([Cl:26])[CH:18]=[CH:17][C:12]=1[C:13]([O:15][CH3:16])=[O:14]>C(O)C.O>[Cl:10][C:11]1[C:20]([CH:21]=[CH:22][C:23](=[N:2][OH:3])[CH3:24])=[C:19]([Cl:26])[CH:18]=[CH:17][C:12]=1[C:13]([O:15][CH3:16])=[O:14]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 54401157Methyl 2,4-dichloro-3-(2-oxobut-3-en-4-yl)benzoate

생성물 1

HCID 73865896Methyl 2,4-dichloro-(2-hydroxyiminobut-3-en-4-yl)benzoate

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

1.8 g (25.9 mmol) of hydroxylamine hydrochloride and 1.5 g (11.0 mmol) of potassium carbonate were added to 5.0 g (18.3 mmol) of methyl 2,4-dichloro-3-(2-oxobut-3-en-4-yl)benzoate in 160 ml of ethanol, and the reaction mixture was admixed with water until a clear solution was obtained. The mixture was heated under reflux for 3 hours and then cooled and the reaction mixture was taken up in 400 ml of water and extracted with ethyl acetate. The combined organic phases were dried and the solvent was removed. Methyl 2,4-dichloro-(2-hydroxyiminobut-3-en-4-yl)benzoate was obtained in quantitative yield.

후처리

  1. customwas obtained
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 3 hours
  4. temperaturecooled
  5. extractionextracted with ethyl acetate
  6. customThe combined organic phases were dried
  7. customthe solvent was removed

출처 및 근거

ORD 기록
ord-297ec87aa4804718b9836e080ac79357
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06165944

반응 노트

불러오는 중…