Hydrochloric Acid → HCID 136388365, 화합물

HRID 432050노트

반응식

HRID 432050 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 136388365HCID 136388365, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7d7c40f548264478a0bd61370a77c91c
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660872B1

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