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

HRID 377542ノート

反応式

HRID 377542 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 ethoxyamine hydrochloride and 1.15 g (0.0085 mol) of finely pulverulent 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 subsequently added. After the mixture was stirred 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 the mixture had been dried and the solvent distilled off, 3.60 g of 2-chloro-3-ethoxyiminomethyl-4-methylsulfonylbenzoic acid were obtained (78% yield).

後処理

  1. customthe solvent was removed
  2. washthe organic phase was washed four times with water
  3. customAfter the mixture had been dried
  4. distillationthe solvent distilled off

出典と根拠

ORDレコード
ord-9f7eb24ff1604ecdaf20b4b7d5c12209
出典データセット
uspto-grants-2000_02
特許番号
US06028035

反応ノート

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