Nitrogen → N,N-Diallylformamide
反応式
[CH:1](OCC)=[O:2].[CH2:6]([NH:9][CH2:10][CH:11]=[CH2:12])[CH:7]=[CH2:8].N#N>>[CH2:6]([N:9]([CH2:10][CH:11]=[CH2:12])[CH:1]=[O:2])[CH:7]=[CH2:8]参加物
4
反応条件
- 温度
- 120 °C
実験手順
Ethyl formate (55.6 g, 750 mmole) and 37.5 g (385 mmole) of N,N-diallyl amine were combined in a 250 mL 3-neck flask equipped with mechanical stirrer, Friedrich condenser, and N2 blanket. The reaction mixture was stirred at reflux temperature (120° C. oil bath) for 24 hours and then sampled by GC to determine if all the N,N-diallylamine was reacted, RT of 0.4 mm. The product was vacuum distilled using a 1-piece apparatus with a fractionation column. The first fraction distilled at 30° C./16 torr. The second fraction N,N-diallylformamide (NDF), distilled at 88°-90° C./10-14 torr. The yield was 95%. Structure was confirmed by NMR.
後処理
- customequipped with mechanical stirrer
- aliquotsampled by GC
- customwas reacted, RT of 0.4 mm
- distillationdistilled
- distillationThe first fraction distilled at 30° C./16 torr
- distillationThe second fraction N,N-diallylformamide (NDF), distilled at 88°-90° C./10-14 torr
出典と根拠
- ORDレコード
- ord-777a03eb8d324563947648e17806b3e4
- 出典データセット
- uspto-grants-1992_10
- 特許番号
- US05155167
反応ノート
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