in hexadeuterioacetone
to cold (-78 °C) soln. of Ti complex (excess) in acetone-d6 added soln. of MeHgCl in acetone-d6 under N2, stirred at -78 °C for 2h, stirred at room temp. for 6 h; monitored by NMR;
参考文献
Puddephatt, Richard J.; Stalteri, Maria A.
Organometallics, 1983 , vol. 2, p. 1400 - 1405
duroquinone or galvinoxyl in further solvent(s)
absence of air and moisture; slow addn. of 1.5 equiv. Bu3SnH to Hg-compd. (both in Bu3SnCl contg. radical inhibitor; 0°C) with simultaneous distn. off of product (vac.); fractional condensation (-40°C, then product at -196°C);
sodium tetrahydroborate in water
addn. of NaBH4 soln. to MeHgCl soln. at pH 4; purging with He or extn. with C6D6 and drying over MgSO4; GLC, atomic absorption detection;
参考文献
Craig, Peter J.; Mennie, Darren; Needham, Michael; Oshah, Naman; Donard, Olivier F.X.; Martin, Fabienne
Journal of Organometallic Chemistry, 1993 , vol. 447, # 1 p. 5 - 8
NaOAc in benzene-d6; acetic acid; benzene
aq. acetic acid; dissoln. od the Hg compound in an acetate buffer (NaOAc/aq. HOAc, pH 3.5), addn. of C6D6 then aq. NaBH4, standing (15 min); sepn. of the benzene layer, drying (MgSO4); spectr. monitoring;
参考文献
Craig, Peter J.; Needham, Michael I.; Ostah, Naaman; Stojak, Grace H.; Symons, Martyn; Teesdale-Spittle, Paul
Journal of the Chemical Society - Dalton Transactions, 1996 , # 2 p. 153 - 156
