Ethyl bromoacetate → Ethyl 2-(1H-1,2,3-triazol-1-YL)acetate
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>[CH2:12]([O:11][C:9](=[O:10])[CH2:8][N:2]1[CH:6]=[CH:5][N:4]=[N:3]1)[CH3:13]参加物
5
実験手順
129.2 g (5.6 mol) sodium are slowly added to 4.0 liters ethanol. 400.0 g (5.6 mol) 1,2,3-1H-triazole are then added and 623 ml (938.2 g, 5.6 mol) ethyl bromoacetate are added dropwise at an internal temperature of 20-25° C. The mixture is stirred at RT for 48 h. The solid which has precipitated out is filtered off, the ethanol is removed in vacuo and the mixture is filtered again. The residue is taken up in ethyl acetate, the mixture is filtered and is concentrated in vacuo again and the residue is purified by distillation over a 30 cm column. The product is obtained at a bath temperature of 140° C., an overhead temperature of 60-115° C. and a pressure of 1 mbar.
後処理
- customThe solid which has precipitated out
- filtrationis filtered off
- customthe ethanol is removed in vacuo
- filtrationthe mixture is filtered again
- filtrationthe mixture is filtered
- concentrationis concentrated in vacuo again
- distillationthe residue is purified by distillation over a 30 cm column
- customThe product is obtained at a bath temperature of 140° C.
- customan overhead temperature of 60-115° C.
出典と根拠
- ORDレコード
- ord-21d40e77427f4d57b248ffd8911826b4
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653111B2
反応ノート
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