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Potassium Hydroxide → 2-(Ethoxycarbonyl)-4-methylpentanoic acid

HRID 1415389
ノート
印刷プレビュー

反応式

HRID 1415389 の反応式
[CH2:1]([O:3][C:4](=[O:15])[CH:5]([CH2:11][CH:12]([CH3:14])[CH3:13])[C:6]([O:8]CC)=[O:7])[CH3:2].[OH-].[K+]>C(O)C>[CH2:1]([O:3][C:4](=[O:15])[CH:5]([CH2:11][CH:12]([CH3:14])[CH3:13])[C:6]([OH:8])=[O:7])[CH3:2]
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 14797Potassium HydroxideHCID 25047Diethyl isobutylmalonate

生成物 1

HCID 101039412-(Ethoxycarbonyl)-4-methylpentanoic acid収率 81.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A total of 21.6 g of isobutylmalonic acid diethyl ester prepared above was dissolved in 100 ml of ethanol and treated dropwise at 0° with a solution of 5.6 g of potassium hydroxide in 100 ml of ethanol. The solution was allowed to stand to neutral pH for 17 hours at 20° and then evaporated under reduced pressure. The residue was dissolved in ice-water and extracted three times with ethyl acetate. The ethyl acetate extracts were rejected. The aqueous phase was acidified with 2-N hydrochloric acid and extracted twice with ethyl acetate. The combined ethyl acetate extracts were washed once with water, dried over magnesium sulfate and evaporated under reduced pressure. There were obtained 15.3 g of colorless isobutylmalonic acid monoethyl ester in the form of a chromatographically pure oil.

後処理

  1. customevaporated under reduced pressure
  2. dissolutionThe residue was dissolved in ice-water
  3. extractionextracted three times with ethyl acetate
  4. extractionextracted twice with ethyl acetate
  5. washThe combined ethyl acetate extracts were washed once with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-2bdd726204614c6e807b8be855ba7de6
出典データセット
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04005073

反応ノート

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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