/Vo e)ruthenium(I) Preption of trichloronítrosylbis(triphenylphosphine)ruthenium(II): The ligand ...
/Vo e)ruthenium(I) Preption of trichloronítrosylbis(triphenylphosphine)ruthenium(II): The ligand NOt is considered to be isoelectronic with the CO ligan Like CO, it shows a variety ich it can bond and react, but it tends to be a little more difficult to make the complex ng the rst place. The method described below is an improvement on earlier methods, usi reagent N-methyl-N-nitroso-p-toluene-sulfonamide. This reagent is also known as Diazaldas it was marketed by Aldrich as the precursor for an easy synthesis of diazomethane Under nitrogen, in a fumehood, reflux and stir1.2g ef triphen elowe 0S in ethanol 15 mL). Add in quick succession solutions of a) 0.2 g of RuCl,.xH,O in ethanol (15 mL(b)0.31 g of N-methyt- N-nitroso-p-toluene-sulfonamide in than 5mL Re ux the combined solutions fora further 5 minutes and attow to coot. Fiterthe crude product, and wash with ethanol, water, ethanol and hexane ( 10 mL in each case). Extract the solid with 5 x 100 mL hot dichloromethane (Warning: use the fume hood. Chlorinated solvents are harmful, and hot solvents have a much higher vapour pressure than those at room temperature). Filter each extraction and combine the fractions. Concentrate on the rotary evaporater, and add sufficient hexane to cause precipitation. Record the ir (as a Nujol mull) and 'P ngrf spectra.24
/Vo e)ruthenium(I) Preption of trichloronítrosylbis(triphenylphosphine)ruthenium(II): The ligand NOt is considered to be isoelectronic with the CO ligan Like CO, it shows a variety ich it can bond and react, but it tends to be a little more difficult to make the complex ng the rst place. The method described below is an improvement on earlier methods, usi reagent N-methyl-N-nitroso-p-toluene-sulfonamide. This reagent is also known as Diazaldas it was marketed by Aldrich as the precursor for an easy synthesis of diazomethane Under nitrogen, in a fumehood, reflux and stir1.2g ef triphen elowe 0S in ethanol 15 mL). Add in quick succession solutions of a) 0.2 g of RuCl,.xH,O in ethanol (15 mL(b)0.31 g of N-methyt- N-nitroso-p-toluene-sulfonamide in than 5mL Re ux the combined solutions fora further 5 minutes and attow to coot. Fiterthe crude product, and wash with ethanol, water, ethanol and hexane ( 10 mL in each case). Extract the solid with 5 x 100 mL hot dichloromethane (Warning: use the fume hood. Chlorinated solvents are harmful, and hot solvents have a much higher vapour pressure than those at room temperature). Filter each extraction and combine the fractions. Concentrate on the rotary evaporater, and add sufficient hexane to cause precipitation. Record the ir (as a Nujol mull) and 'P ngrf spectra.24