Water → Diethyl {[di(prop-2-en-1-yl)amino]methyl}phosphonate
反応式
C(NC[CH2:6][P:7](=[O:14])([O:11][CH2:12][CH3:13])[O:8][CH2:9][CH3:10])C=C.C([N:17]([CH2:20][CH3:21])CC)C.[CH2:22](Br)[CH:23]=[CH2:24].O.[CH2:27](OCC)C>>[CH2:22]([N:17]([CH2:6][P:7](=[O:14])([O:8][CH2:9][CH3:10])[O:11][CH2:12][CH3:13])[CH2:20][CH:21]=[CH2:27])[CH:23]=[CH2:24]参加物
6
実験手順
0.60 g (2.9 mmole) of diethyl allylaminoethylphosphonate was dissolved in 50 ml dry diethyl ether, and 1.17 g (11.6 mmole) triethylamine was added. After 15 minutes of stirring at room temperature, 1.40 g of allylbromide was added dropwise. The mixture was refluxed during 4 days. 50 ml of water was added to the mixture and was subsequently extracted three times with 50 ml CH2Cl2. The organic layers were combined and dried with MgSO4. After filtering MgSO4 and subsequent evaporation of the solvent, the resulting product was further purified with high vacuum distillation, providing 0,6 gram (2,4 mmole, 84% yield) diethyl diallylaminomethylphosphonate having a boiling point of 65° C. under a reduced pressure of 0.1 mbar. This product was further characterised by the following spectra: