Potassium Carbonate → 2-Chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoic acid

HRID 1368814노트

반응식

HRID 1368814 반응식
Cl.[CH2:2]([O:4][NH2:5])[CH3:3].C(=O)([O-])[O-].[K+].[K+].[Cl:12][C:13]1[C:21]([CH:22]=O)=[C:20]([S:24]([CH3:27])(=[O:26])=[O:25])[CH:19]=[CH:18][C:14]=1[C:15]([OH:17])=[O:16]>CO>[Cl:12][C:13]1[C:21]([CH:22]=[N:5][O:4][CH2:2][CH3:3])=[C:20]([S:24]([CH3:27])(=[O:26])=[O:25])[CH:19]=[CH:18][C:14]=1[C:15]([OH:17])=[O:16]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 76850O-ethylhydroxylamine hydrochlorideHCID 185174222-Chloro-3-formyl-4-methylsulfonylbenzoic acid

생성물 1

HCID 541651472-Chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoic acid수율 78.5%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

1.63 g (0.017 mol) of O-ethylhydroxylamine hydrochloride and 1.15 g (0.0085 mol) of finely powdered potassium carbonate were stirred for 1 hour in 60 ml of dry methanol. 4.00 g (0.015 mol) of 2-chloro-3-formyl-4-methylsulfonylbenzoic acid in 40 ml of methanol were then added. After stirring for 12 hours at room temperature, the solvent was removed, the residue was taken up in ethyl acetate and the organic phase was washed four times with water. After drying and removal of the solvent by distillation, 3.60 g of 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoic acid (78% yield) were obtained.

후처리

  1. customthe solvent was removed
  2. washthe organic phase was washed four times with water
  3. customAfter drying
  4. customremoval of the solvent
  5. distillationby distillation

출처 및 근거

ORD 기록
ord-8cede7a66126465d97f5c16195d32a9e
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06576596B1

반응 노트

불러오는 중…