Hydrochloric Acid → HCID 136388365、化合物

HRID 432050ノート

反応式

HRID 432050 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].Cl.[NH2:15][OH:16].O.Cl>CO>[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[N:15][OH:16])[C:9]([O:11][CH3:12])=[O:10]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 182159Benzeneacetic acid, 2-hydroxy-alpha-oxo-, methyl esterHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 136388365HCID 136388365、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3.3 g (0.016 mol) of methyl 2-hydroxyphenylglyoxylate (HPLC: 88%, log p=1.87) (Example VI-1a) and 1.3 g (0.019 mol) of hydroxylamine hydrochloride in 50 ml of methanol are heated under reflux for one hour. The reaction mixture is poured into water, acidified with 2N hydrochloric acid and extracted with diethyl ether, the organic phase is dried over sodium sulphate and the solvent is distilled off under reduced pressure. This gives 2.4 g of crude product which, according to HPLC, contains 17.1% of methyl E-2-(2-hydroxyphenyl)-2-hydroxyimino-acetate of log p=0.95 and 68.9% of methyl Z-2-(2-hydroxyphenyl)-2-hydroxyimino-acetate of log p=1.68.

後処理

  1. temperatureunder reflux for one hour
  2. extractionextracted 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-7d7c40f548264478a0bd61370a77c91c
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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