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Sodium Hydroxide → (2,6-Diethyl-4-methylphenyl)glyoxylic acid

HRID 579217
ノート
印刷プレビュー

反応式

HRID 579217 の反応式
[CH2:1]([C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH2:10][CH3:11])[C:4]=1[C:12](=[O:18])[C:13]([O:15]CC)=[O:14])[CH3:2].[OH-].[Na+]>O1CCCC1>[CH2:10]([C:5]1[CH:6]=[C:7]([CH3:9])[CH:8]=[C:3]([CH2:1][CH3:2])[C:4]=1[C:12](=[O:18])[C:13]([OH:15])=[O:14])[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 56942718Ethyl (2,6-diethyl-4-methylphenyl)glyoxylate

生成物 1

HCID 56942555(2,6-Diethyl-4-methylphenyl)glyoxylic acid収率 58.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a 3 L volume four-necked flask, ethyl 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetate (9-a) (320.82 g) and tetrahydrofuran (600 ml) were added at room temperature and cooled. 10.7% by weight of aqueous sodium hydroxide solution (900 ml) was added dropwise at 10° C. over 2 hours. The resulting mixture was stirred at room temperature for 1 hour. After the organic solvent was removed under reduced pressure, tert-butyl methyl ether was added to the aqueous layer to wash. After the organic layer was removed, to the aqueous layer was added dropwise concentrated hydrochloric acid (180 ml), and extracted with tert-butyl methyl ether. The organic layer was concentrated under reduced pressure to give 166.55 g of 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetic acid (8-a).

後処理

  1. temperaturecooled
  2. customAfter the organic solvent was removed under reduced pressure, tert-butyl methyl ether
  3. additionwas added to the aqueous layer
  4. washto wash
  5. customAfter the organic layer was removed, to the aqueous layer
  6. additionwas added dropwise concentrated hydrochloric acid (180 ml)
  7. extractionextracted with tert-butyl methyl ether
  8. concentrationThe organic layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-23e01e95bf0a4876a9a78c670723f063
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09040709B2

反応ノート

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