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Ethyl bromoacetate → Ethyl 2-(1H-1,2,3-triazol-1-YL)acetate

HRID 562444
ノート
印刷プレビュー

反応式

HRID 562444 の反応式
[Na].[NH:2]1[CH:6]=[CH:5][N:4]=[N:3]1.Br[CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10]>C(O)C>[N:2]1([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:6]=[CH:5][N:4]=[N:3]1
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 7748Ethyl bromoacetateHCID 5360545SodiumHCID 178418936HCID 178418936、化合物

生成物 1

HCID 10103365Ethyl 2-(1H-1,2,3-triazol-1-YL)acetate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

129.2 g (5.6 mmol) of sodium are added slowly to 4.0 litres of ethanol. 400.0 g (5.6 mol) of 1,2,3-1H-triazole are then added, and 623 ml (938.2 g, 5.6 mol) of ethyl bromoacetate are added dropwise at an internal temperature of 20-25° C. The mixture is stirred at RT for 48 h. The precipitated solid is filtered off, the ethanol is removed under reduced pressure and the mixture is filtered again. The residue is taken up in ethyl acetate, filtered, again concentrated under reduced pressure and purified by distillation on a 30 cm column. The product is obtained at a bath temperature of 140° C., a head temperature of 60-115° C. and a pressure of 1 mbar. Yield: 440.0 g (50% of theory)

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

後処理

  1. filtrationThe precipitated solid is filtered off
  2. customthe ethanol is removed under reduced pressure
  3. filtrationthe mixture is filtered again
  4. filtrationfiltered
  5. concentrationagain concentrated under reduced pressure
  6. distillationpurified by distillation on a 30 cm column
  7. customThe product is obtained at a bath temperature of 140° C.
  8. customa head temperature of 60-115° C.

出典と根拠

ORDレコード
ord-951eeb148d06444b83c2c93ba618087f
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08067407B2

反応ノート

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