Methanol → (4-Methoxyphenyl)glyoxylic acid

HRID 1859306ノート

反応式

HRID 1859306 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 584714(4-Methoxyphenyl)glyoxylic acid

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1ed1c0550bdc4d9db12c472062f711f3
出典データセット
uspto-grants-2000_11
特許番号
US06153768

反応ノート

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