反应 #2460323

反应方程式

2, 5-dibromo-α,α′-dibromo-p-xylene

2,5-dibromo-α,α′-dibromo-p-xylene

triethyl phosphite

→

product

收率 82.2%

tetraethyl 2,5-dibromo-p-xylenebisphosphonate

收率 82.2%

反应条件

后处理

1. 1
   其他The excess triethyl phosphite was removed under reduced pressure, 60 ml of hexanes
2. 2
   workup.ADDITIONwas added
3. 3
   其他white solid was formed
4. 4
   过滤The solid was collected by filtration
5. 5
   洗涤washed three times with 20 ml of hexanes

实验过程

The mixture of 2, 5-dibromo-α,α′-dibromo-p-xylene (67) (7.58 g, 0.018 mol) and triethyl phosphite (60 ml) was refluxed at 180° C. overnight. The excess triethyl phosphite was removed under reduced pressure, 60 ml of hexanes was added, and white solid was formed. The solid was collected by filtration, washed three times with 20 ml of hexanes and gave 7.93 g (82.2%) of product.1H NMR (CDCl3, 500 MHz) δppm: 7.62 (s, 2H, Ar—H), 4.06 (m, 8H, CH2), 3.32 (d, J=20.5 Hz, 4H, CH2), 1.28 (t, J=7.0 Hz, 12H, CH3)13C NMR (CDCl3, 125.7 MHz) δppm: 135.2, 132.5, 123.6, 62.35, 62.32, 33.4, 32.2, 16.31, 16.28GC-MS (relative intensity %): 491 (M+, <5%).

来源