3-CHLOROPROPYLTRIS(TRIMETHYLSILOXY)SILANE

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

実験手順: To 186.3 grams (0.5 moles) of the tris-trimethylsiloxy-3-chloropropylsilane in 250 gm. of 2-butanone is added 71.5 grams (0.5 moles) of methyloctylamine. The mixture is heated in an autoclave under 200 psi. nitrogen to 130° C. for 18 hours. The 2-butonone is removed from the product by distillation and the residue is added to two liters of hexane. An excess of trimethylamine (anhydrous gas) is added and the mixture is allowed to stir for 16 hours. Filtration to remove the trimethylamine hydrochloride salt, and short path distillation of the filtrate yields tris-trimethylsiloxy-3-octylmethylaminopropylsilane. The mixture is heated in an autoclave under 200 psi The 2-butonone is removed from the product by distillation the residue is added to two liters of hexane An excess of trimethylamine (anhydrous gas) is added Filtration to remove the trimethylamine hydrochloride salt, and short path distillation of the filtrate

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

実験手順: Gamma-chloropropyltrichlorosilane (21.2 g., 0.1 mole) is dissolved in 200 ml. of dry ether and an ether slurry of (33.6g, 0.3 mole) sodium trimethylsilanoate, (CH3)3SiONa, is added in small portions. The mixture is allowed to stand for 12 hours and is then refluxed for an additional 3 hours. Filtration of the sodium chloride and removal of the ether from the filtrate leaves gamma-chloropropyltris-trimethylsiloxysilane. is then refluxed for an additional 3 hours Filtration of the sodium chloride and removal of the ether from the filtrate

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

実験手順: Gamma-chloropropyltrichlorosilane (21.2 g., 0.1 mole) is dissolved in 200 ml. of dry ether and an ether slurry of (33.6g, 0.3 mole) sodium trimethylsilanoate, (CH3)3SiONa, is added in small portions. The mixture is allowed to stand for 12 hours and is then refluxed for an additional 3 hours. Filtration of the sodium chloride and removal of the ether from the filtrate leaves gamma-chloropropyltris-trimethylsiloxysilane. is then refluxed for an additional 3 hours Filtration of the sodium chloride and removal of the ether from the filtrate

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

実験手順: 90 g of 3-chloropropyltris(trimethylsiloxy)silane (27) (Chem. Abstracts No. 18077-31-1) and 105.22 g of sodium iodide are added to 250 ml of acetone and stirred for 24 hours at reflux. The acetone is evaporated and the residue taken up in methylene chloride. The organic phase is washed with water, dried and evaporated. 89 g of the desired 3-iodopropyl-tris(trimethylsiloxy)silane (28) are obtained; 1H-NMR (ppm, CDCl3): 3.12 2H t, 1.75 2H txt, 0.43 2H t, 0 27H s. at reflux The acetone is evaporated The organic phase is washed with water dried evaporated

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

実験手順: To 186.3 grams (0.5 moles) of the tris-trimethylsiloxy-3-chloropropylsilane in 250 gm. of 2-butanone is added 71.5 grams (0.5 moles) of methyloctylamine. The mixture is heated in an autoclave under 200 psi. nitrogen to 130° C. for 18 hours. The 2-butonone is removed from the product by distillation and the residue is added to two liters of hexane. An excess of trimethylamine (anhydrous gas) is added and the mixture is allowed to stir for 16 hours. Filtration to remove the trimethylamine hydrochloride salt, and short path distillation of the filtrate yields tris-trimethylsiloxy-3-octylmethylaminopropylsilane. The mixture is heated in an autoclave under 200 psi The 2-butonone is removed from the product by distillation the residue is added to two liters of hexane An excess of trimethylamine (anhydrous gas) is added Filtration to remove the trimethylamine hydrochloride salt, and short path distillation of the filtrate

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

実験手順: Gamma-chloropropyltrichlorosilane (21.2 g., 0.1 mole) is dissolved in 200 ml. of dry ether and an ether slurry of (33.6g, 0.3 mole) sodium trimethylsilanoate, (CH3)3SiONa, is added in small portions. The mixture is allowed to stand for 12 hours and is then refluxed for an additional 3 hours. Filtration of the sodium chloride and removal of the ether from the filtrate leaves gamma-chloropropyltris-trimethylsiloxysilane. is then refluxed for an additional 3 hours Filtration of the sodium chloride and removal of the ether from the filtrate