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Lithium iodide → 2-Chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoic acid

HRID 1368816
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HRID 1368816 반응식
[Cl:1][C:2]1[C:11]([CH:12]=[N:13][O:14][CH2:15][CH3:16])=[C:10]([S:17]([CH3:20])(=[O:19])=[O:18])[CH:9]=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].[I-].[Li+]>N1C=CC=CC=1>[Cl:1][C:2]1[C:11]([CH:12]=[N:13][O:14][CH2:15][CH3:16])=[C:10]([S:17]([CH3:20])(=[O:19])=[O:18])[CH:9]=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 66321Lithium iodideHCID 54512790Methyl 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoate

생성물 1

HCID 541651472-Chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoic acid수율 89%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 4.37 g (0.0137 mol) of methyl 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoate was slowly added dropwise to 7.29 g (0.055 mol) of lithium iodide in 50 ml of dry pyridine. After stirring for 2 hours at reflux, the reaction mixture was cooled and the solvent was removed under reduced pressure. The residue was taken up in water and adjusted to pH=1-2 with dilute hydrochloric acid. The aqueous phase was extracted with ethyl acetate and the combined organic phases were washed with water, dried and concentrated under reduced pressure. 3.70 g of 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoic acid were obtained. (Yield 89%).

후처리

  1. temperatureat reflux
  2. temperaturethe reaction mixture was cooled
  3. customthe solvent was removed under reduced pressure
  4. extractionThe aqueous phase was extracted with ethyl acetate
  5. washthe combined organic phases were washed with water
  6. customdried
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f7115e2b1be940028bfffa6655a5dcaf
출처 데이터셋
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06576596B1

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