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

HRID 1368814ノート

反応式

HRID 1368814 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: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]

参加物

5

反応物 3

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

生成物 1

HCID 541651472-Chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoic acid収率 78.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8cede7a66126465d97f5c16195d32a9e
出典データセット
uspto-grants-2003_06
特許番号
US06576596B1

反応ノート

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