Water → HCID 136127060, 화합물

HRID 432053노트

반응식

HRID 432053 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].[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 136127060HCID 136127060, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-39f053a2bb5249da8703107218e8f589
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660872B1

반응 노트

불러오는 중…