反应详情

2.0×10-3 mol of CH3OCH2CH2OLi in solution in THF are introduced under nitrogen atmosphere into a predried round bottom flask. 100 ml of predried THF are added followed, with stirring, dropwise, by 1.0×10-3 mol of (Ph)2CHLi in 0.2-molar solution in THF. The mixture is cooled to a temperature of -78° C. with a mixture of acetone and solid carbon dioxide, followed by the addition, still at -78° C., of 0.048 mol of 2-ethylhexyl acrylate previously stirred for 48 hours over calcium hydride, distilled and then treated over fluorenyllithium until the appearance of a yellow colour and distilled over triethylaluminium immediately before the polymerisation. After 10 minutes the reaction is stopped by addition of 5 ml of acidified methanol and the solvent is then stripped off. An ethylhexyl acrylate polymer is obtained in a 95% yield. Analysis of the polymer by GPC shows the following characteristics:

1. distillationdistilled
2. additiontreated over fluorenyllithium until the appearance of a yellow colour
3. distillationdistilled over triethylaluminium immediately before the polymerisation
4. additionAfter 10 minutes the reaction is stopped by addition of 5 ml of acidified methanol