ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Ethanol → 4-Fluoro-3,3-dimethyl-2-oxobutanoic acid

HRID 520357
ノート
印刷プレビュー

反応式

HRID 520357 の反応式
[F:1][CH2:2][C:3]([CH3:8])([CH3:7])[C:4](=[O:6])[CH3:5].[OH-:9].[Na+].[Mn]([O-])(=O)(=O)=[O:12].[K+].CCO>O>[F:1][CH2:2][C:3]([CH3:8])([CH3:7])[C:4](=[O:6])[C:5]([OH:12])=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 516875Potassium PermanganateHCID 130194414-Fluoro-3,3-dimethylbutan-2-one

生成物 1

HCID 866900774-Fluoro-3,3-dimethyl-2-oxobutanoic acid収率 44.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a vigorous stirring mixture of 4-fluoro-3,3-dimethylbutan-2-one (4.1 g, 34.7 mmol) in water (50 mL) and NaOH (7 mL, 70.0 mmol) cooled in an ice-acetone bath was added portionwise potassium permanganate (9.87 g, 62.5 mmol). The inner temperature was controlled between −3 to 2° C. during the addition process. Upon the completion of the addition, the reaction mixture was stirred in the ice-acetone bath for 6 hrs and then allowed to warm up. EtOH (5 mL) was added and the reaction mixture was stirred for another 15 min. The reaction mixture was filtered and the solid was washed with water (˜80 mL). The filtration was acidified with 6 N HCl, and extracted with EtOAc. The combined extracts were washed with 1N HCl, sat. NaCl, dried (Na2SO4), filtered and concentrated to yield 4-fluoro-3,3-dimethyl-2-oxobutanoic acid (2.3 g).

後処理

  1. temperaturecooled in an ice-acetone bath
  2. customwas controlled between −3 to 2° C. during the addition process
  3. additionUpon the completion of the addition
  4. temperatureto warm up
  5. filtrationThe reaction mixture was filtered
  6. washthe solid was washed with water (˜80 mL)
  7. filtrationThe filtration
  8. extractionextracted with EtOAc
  9. washThe combined extracts were washed with 1N HCl, sat. NaCl
  10. dry with materialdried (Na2SO4)
  11. filtrationfiltered
  12. concentrationconcentrated

出典と根拠

ORDレコード
ord-add77a6f154e4496915beb8231a3899d
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09326973B2

反応ノート

読み込み中…

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