3-chloropropyl-methoxy-dimethylsilane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under Ar, a solution of CH3OSi(CH3)2(CH2)3Cl (10.0 g, 59.3 mmol), CH3NHCH2CH2N(CH3)2 (10.0 g, 98.2 mmol) and methanol (5.0 mL) is refluxed for 22 h and then concentrated with a rotary evaporator (about 10 Torr, about 45 ° C.). The concentrate is diluted with ether (50 mL) and filtered. The solid is washed with ether (50 mL), the washings and the filtrate are combined, and the resulting solution is concentrated with a rotary evaporator (about 60 Torr, about 30 ° C.). The concentrate is filtered and the solid is washed with ether (10 mL). The washings and the filtrate are combined, and the resulting solution is concentrated with a rotary evaporator (about 60 Torr, about 30° C.). The resultant ligand, CH3OSi(CH3)2(CH2)3N(CH3)(CH2)2N(CH3)2, having the form of a light yellow liquid, is weighed (8.46 g, 36.4 mmol, 61%). concentrated with a rotary evaporator (about 10 Torr, about 45 ° C.) The concentrate is diluted with ether (50 mL) filtered The solid is washed with ether (50 mL) the resulting solution is concentrated with a rotary evaporator (about 60 Torr, about 30 ° C.) The concentrate is filtered the solid is washed with ether (10 mL) the resulting solution is concentrated with a rotary evaporator (about 60 Torr, about 30° C.)