Methanol → (4-Methoxyphenyl)glyoxylic acid

HRID 1859306노트

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HRID 1859306 반응식
C([O:3][C:4](=[O:15])[C:5]([C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=1)=[O:6])C.CO>[OH-].[Na+]>[CH3:14][O:13][C:10]1[CH:9]=[CH:8][C:7]([C:5](=[O:6])[C:4]([OH:15])=[O:3])=[CH:12][CH:11]=1

참가 물질

4

반응물 2

HCID 887MethanolHCID 2758864Ethyl 2-(4-methoxyphenyl)-2-oxoacetate

생성물 1

HCID 584714(4-Methoxyphenyl)glyoxylic acid

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

반응 조건

온도
80 °C

실험 절차

4-Methoxyphenylglyoxylic ethyl ester obtained in Example 20 was dissolved in 20% sodium hydroxide (60 mg) and methanol (600 ml) and then stirred for 3 hours with heating at 80° C. When the reaction is completed, the reaction solution was extracted with diethyl ether (200 mg) and the obtained aqueous solution was acidified (pH 1-2) with hydrochloric acid. The resulting aqueous acidic solution was extracted with dichloromethane, and the extract was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to remove the organic solvent to obtain 34.63 g (yield in two reaction steps: 43%) of the title compound as a pale violet solid.

후처리

  1. extractionthe reaction solution was extracted with diethyl ether (200 mg)
  2. extractionThe resulting aqueous acidic solution was extracted with dichloromethane
  3. dry with materialthe extract was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto remove the organic solvent
  6. customto obtain

출처 및 근거

ORD 기록
ord-1ed1c0550bdc4d9db12c472062f711f3
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06153768

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