Water → 2-Methoxyethyl alpha-(hydroxyimino)-2-phenylacetate

HRID 393135노트

반응식

HRID 393135 반응식
[C:1]1([C:7](=O)[C:8]([O:10][CH2:11][CH2:12][O:13][CH3:14])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[OH:17][NH3+:18].C(OCC)(=O)C.O>N1C=CC=CC=1>[OH:17][N:18]=[C:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[C:8]([O:10][CH2:11][CH2:12][O:13][CH3:14])=[O:9]

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 134616742-Methoxyethyl 2-oxo-2-phenylacetateHCID 22029257Hydroxyammonium hydrochloride

생성물 1

HCID 739911462-Methoxyethyl alpha-(hydroxyimino)-2-phenylacetate수율 102.9%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

61.7 g (0.296 mol) of 2-methoxyethyl phenylglyoxalate are dissolved in 360 ml pyridine. 22.7 g (0.0.326 mol) of hydroxylammonium hydrochloride are added in portions to this solution. When the addition is complete, the reaction mixture is stirred at room temperature for 2 hours. After addition of ethyl acetate and water, the organic layer is separated, washed with diluted HCl and water and dried over magnesium sulfate. Evaporation of the solvent gives 68 g (100%) of crude 2-methoxyethyl α-(hydroxyimino)-2-phenylacetate as a slightly brownish liquid. This compound is used without further purification in the next step.

후처리

  1. additionWhen the addition
  2. customthe organic layer is separated
  3. washwashed with diluted HCl and water
  4. dry with materialdried over magnesium sulfate
  5. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-153d0b723769488b82a655356e886643
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06806024B1

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