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

HRID 1368816
ノート
印刷プレビュー

反応式

HRID 1368816 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 541651472-Chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoic acid収率 89%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-f7115e2b1be940028bfffa6655a5dcaf
出典データセット
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06576596B1

反応ノート

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