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Potassium Carbonate → Methyl 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoate

HRID 1368815
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HRID 1368815 반응식
Cl.[CH2:2]([O:4][NH2:5])[CH3:3].C(=O)([O-])[O-].[K+].[K+].[Cl:12][C:13]1[C:22]([CH:23]=O)=[C:21]([S:25]([CH3:28])(=[O:27])=[O:26])[CH:20]=[CH:19][C:14]=1[C:15]([O:17][CH3:18])=[O:16]>CO>[Cl:12][C:13]1[C:22]([CH:23]=[N:5][O:4][CH2:2][CH3:3])=[C:21]([S:25]([CH3:28])(=[O:27])=[O:26])[CH:20]=[CH:19][C:14]=1[C:15]([O:17][CH3:18])=[O:16]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 76850O-ethylhydroxylamine hydrochlorideHCID 18517410Methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate

생성물 1

HCID 54512790Methyl 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoate수율 88.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1.90 g (0.0195 mol) of O-ethylhydroxylamine hydrochloride and 1.35 g (0.0097 mol) of finely powdered potassium carbonate were stirred for 1 hour at room temperature in 60 ml of dry methanol, and 4.90 g (0.0177 mol) of methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate were then added. After stirring for 8 hours at room temperature, the solvent was removed, the residue was taken up in ethyl acetate and the organic phase was washed with water until neutral, dried and concentrated under reduced pressure. 5.00 g of methyl 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoate were obtained. (Yield 88%).

후처리

  1. customthe solvent was removed
  2. washthe organic phase was washed with water until neutral,
  3. customdried
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e002bb363c9643ca8f2f5247818a8978
출처 데이터셋
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06576596B1

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