We're trying to follow the old Chisholm prep from 1981 (http://dx.doi.org/10.1021%2Fic50220a049) and are getting super low yields. Any words of advice?
Ta(NMe2)5 + 2 TMSCl --> [TaCl2(NMe2)3]2 + 2 TMSNMe2
we're being quite rigorous with technique; I saw the student set up the reaction. Vac transfer of the TMSCl was fine. We got product, but only about 10% yield. Lots of stuff remaining in solution. We are using a slight excess of TMSCl, but perhaps we need more?
thanks in advance, any lurkers out there,