Triethyl phosphite → HCID 86600084、化合物
反応式
[Br:1][C:2]1[CH:7]=[C:6]([CH2:8]Br)[CH:5]=[CH:4][C:3]=1[CH2:10]Br.[P:12]([O:19][CH2:20][CH3:21])([O:16]CC)[O:13][CH2:14][CH3:15]>>[Br:1][C:2]1([P:12]([O:13][CH2:14][CH3:15])(=[O:16])[O:19][CH2:20][CH3:21])[C:7]([P:12]([O:19][CH2:20][CH3:21])(=[O:16])[O:13][CH2:14][CH3:15])=[C:6]([CH3:8])[CH:5]=[CH:4][CH:3]1[CH3:10]参加物
3
反応条件
- 温度
- 180 °C
実験手順
The mixture of 2-bromo-α,α′-dibromo-p-xylene (68) (14.43 g, 0.042 mol) and triethyl phosphite (145 ml) was refluxed at 180° C. overnight. The excess triethyl phosphite was removed under reduced pressure, 60 ml of hexanes was added, the mixture was cooled at −78 ° C. and white solid was formed on vigorous stirring. The solid was collected by rapid filtration, washed three times with 20 ml of cool hexanes, dried in vacuo and isolated in 14.0 g (72.7%) yield as light yellow oil.1H NMR (CDCl3, 500 MHz) δppm: 7.51 (s, br, 1H), 7.40 (dd, 3J=7.7 Hz, 4J=2.2 Hz, 1H), 7.21 (d, 3J=8.0 Hz, 1H) 4.04 (m, 8H, CH2), 3.38 (d, J=21.5 Hz, 2H, CH2), 3.09 (d, J=21.5 Hz, 2H, CH2), 1.25 (m, 12H, CH3).