Jozef Hodyl PhD Thesis - Theses - Flinders University

To a suspension of 33 (1.48 g, 1.1 mmol g -1 ) in dry toluene (20 cm 3 )trimethylchlorosilane (TMCS), 84 (5.92 g, 54.5 mmol) was added and the mixturewas heated at reflux temperature for 3 h. After cooling the suspension it was stirredat ambient temperature overnight. The solid was then filtered and washed withtoluene (100 cm 3 ) and de-ionised water (200 cm 3 ). The resultant solid 85 was thendried under vacuum for 24 h and stored in a desiccator.Si-GPS-Trac(endcapped), 89Preparation of this material was by the same method as used for 43, but using 85(1.3 g) and 46 (2.23 g, 3.58 mmol).Si-GPS-Trac(230-400), 87This material was prepared by an analogous method to, 33, but using 80 (1.0 g,0.88 mmol -1 ) and 46 (1.4 g, 2.2 mmol). Microanalysis gave 17.44% C, 2.57% H and1.52% N corresponding to a loading of 0.27 mmol g -1 of material.Si-GPDMS 8383This material was prepared by a procedure analogous to that used for 33 with149