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Acetonitrile → Acetic acid, azido-, ethyl ester

HRID 67700
ノート
印刷プレビュー

反応式

HRID 67700 の反応式
Cl[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].C(#N)C.[N-:11]=[N+:12]=[N-:13].[Na+]>O>[N:11]([CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4])=[N+:12]=[N-:13]
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 6342AcetonitrileHCID 7751Ethyl chloroacetateHCID 33557Sodium Azide

生成物 1

HCID 69480Acetic acid, azido-, ethyl ester収率 76%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 490 g. (4 moles) of ethyl chloroacetate in 1500 ml. of acetonitrile were added 260 g. (4 moles) of sodium azide, and the mixture was heated at the reflux temperature for 20 hours. After heating, the reaction mixture was poured into 1 liter of water with stirring for 1/2 hour. The organic phase was separated from the aqueous phase and evaporated in vacuo to dryness. The yellow residual oil was dissolved in 1200 ml. of diethyl ether and the solution was dried over magnesium sulfate. Evaporation of the diethyl ether in vacuo gave 391 g. (76% yield) of ethyl azidoacetate.

後処理

  1. temperatureAfter heating
  2. customThe organic phase was separated from the aqueous phase
  3. customevaporated in vacuo to dryness
  4. dissolutionThe yellow residual oil was dissolved in 1200 ml
  5. dry with materialof diethyl ether and the solution was dried over magnesium sulfate
  6. customEvaporation of the diethyl ether in vacuo
  7. customgave 391 g

出典と根拠

ORDレコード
ord-2e24f4cc5a0741c6bf36e84fedfc7470
出典データセット
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04346076

反応ノート

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