Nitrogen → N,N-Diallylformamide

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[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]

참가 물질

반응물 3

HCID 947Nitrogen

HCID 8025Ethyl formate

HCID 31279Diallylamine2회

생성물 1

HCID 246338N,N-Diallylformamide수율 95%

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온도: 120 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록: ord-777a03eb8d324563947648e17806b3e4
출처 데이터셋: uspto-grants-1992_10
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05155167

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