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

HRID 1368815
ノート
印刷プレビュー

反応式

HRID 1368815 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 54512790Methyl 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoate収率 88.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-e002bb363c9643ca8f2f5247818a8978
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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