Water → HCID 136127060、化合物

HRID 432053ノート

反応式

HRID 432053 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=O)[C:9]([O:11][CH3:12])=[O:10].[CH3:14][O:15][NH3+:16].[Cl-].O>CO>[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[N:16][O:15][CH3:14])[C:9]([O:11][CH3:12])=[O:10]

参加物

5

反応物 3

HCID 962WaterHCID 11639O-methylhydroxylammonium chlorideHCID 182159Benzeneacetic acid, 2-hydroxy-alpha-oxo-, methyl ester

生成物 1

HCID 136127060HCID 136127060、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

10.4 g (0.0533 mol) of methyl 2-hydroxyphenylglyoxylate (HPLC: 92.4%, log p=1.87) from process step 2 and 7.4 g (0.089 mol) of 0-methylhydroxylamine hydrochloride in 150 ml of methanol are boiled under reflux for three hours. The reaction mixture is poured into water, the product is extracted with diethyl ether, the organic phase is dried over sodium sulphate and the solvent is distilled off under reduced pressure. This gives 8.2 g of crude product which, according to HPLC, contains 17.2% methyl E-2-(2-hydroxyphenyl)-2-methoxyimino-acetate of log p=1.48 and 65.4% methyl Z-2-(2-hydroxyphenyl)-2-methoxyimino-acetate of log p=2.38.

後処理

  1. temperatureunder reflux for three hours
  2. extractionthe product is extracted with diethyl ether
  3. dry with materialthe organic phase is dried over sodium sulphate
  4. distillationthe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-39f053a2bb5249da8703107218e8f589
出典データセット
uspto-grants-2003_12
特許番号
US06660872B1

反応ノート

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