Water → 4-Azidobutanoic Acid

HRID 964291ノート

反応式

HRID 964291 の反応式
[N:1]([CH2:4][CH2:5][CH2:6][C:7]([O:9]CC)=[O:8])=[N+:2]=[N-:3].[OH-].[K+].O>CO>[N:1]([CH2:4][CH2:5][CH2:6][C:7]([OH:9])=[O:8])=[N+:2]=[N-:3]

参加物

5

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 12382175Ethyl 4-azidobutanoate

生成物 1

HCID 118047834-Azidobutanoic Acid収率 80%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

Ethyl 4-azidobutyrate (8.06 g, 51.3 mmol) and KOH (14.4 g, 0.256 mol) were dissolved into a mixture of 100 ml of water and 120 ml of MeOH. The solution was stirred at 0° C. for 2 hrs and then MeOH was removed in vacuo. The aqueous layer was extracted by CHCl3 (50 ml), acidified to pH=1 by 2N aqueous HCl and extracted by Et2O (2×100 ml). The organic layers were combined, washed with water (100 ml) and dried over Na2SO4. After filtration and evaporation of solvent, 4-azidobutyric acid (5.30 g, 80%) was obtained as a colorless oil.

後処理

  1. customMeOH was removed in vacuo
  2. extractionThe aqueous layer was extracted by CHCl3 (50 ml)
  3. extractionextracted by Et2O (2×100 ml)
  4. washwashed with water (100 ml)
  5. dry with materialdried over Na2SO4
  6. filtrationAfter filtration and evaporation of solvent

出典と根拠

ORDレコード
ord-6e773e57ee114b6bb2f852ce9a11ba7d
出典データセット
uspto-grants-1998_06
特許番号
US05767131

反応ノート

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