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Methanol → Benzeneacetic acid, 2-hydroxy-alpha-oxo-, methyl ester

HRID 432052
ノート
印刷プレビュー

反応式

HRID 432052 の反応式
[C:1](Cl)(=[O:3])C.C[OH:6].[O:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[C:9](=[O:16])[C:8]1=NO>CC(C)=O>[OH:7][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[C:9](=[O:16])[C:8]([O:3][CH3:1])=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 6367Acetyl chlorideHCID 178516824HCID 178516824、化合物

生成物 1

HCID 182159Benzeneacetic acid, 2-hydroxy-alpha-oxo-, methyl ester

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

27 g of acetyl chloride (0.344 mol) are added dropwise to a mixture of 245 ml of methanol and 245 ml of acetone. 20 g (0.123 mol) of benzofuran-2,3-dione 2-oxime are dissolved in this mixture and the mixture is subsequently heated under reflux for 1 hour. The solvent is distilled off under reduced pressure, the residue 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 20.8 g of crude product which, according to HPLC, contains 92.4% methyl 2-hydroxyphenylglyoxylate of log p=1.87.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturethe mixture is subsequently heated
  2. temperatureunder reflux for 1 hour
  3. distillationThe solvent is distilled off under reduced pressure
  4. additionthe residue is poured into water
  5. extractionthe product is extracted with diethyl ether
  6. dry with materialthe organic phase is dried over sodium sulphate
  7. distillationthe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-3ea6f16492de4ba69a52bca564e98c13
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06660872B1

反応ノート

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