Technology Process of Arsine, diphenyl[(triphenylplumbyl)methyl]-
There total 2 articles about Arsine, diphenyl[(triphenylplumbyl)methyl]- which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
water; lithium;
In
tetrahydrofuran;
byproducts: (C6H5)2AsCH3, Pb(C6H5)4; refluxing of Ph2AsCl in THF with Li wire under N2 for 4 h; filtration of the red cloudy soln. (glass fibre); dropwise addn. of ICH2PbPh3 in THFat 0°C; warming to room temp.; hydrolysis with H2O;; extn. with CHCl3 two times; drying of the extract over Na2SO4; evapn.; column chromy. (Al2O3, benzine/ether (10:1)), isolation of the second fraction;;
- Guidance literature:
-
With
water;
In
diethyl ether;
addn. of Ph2AsCl in ether to a soln. of LiCH2PbPh3 (prepd. by I/Li exchange with BuLi from Ph3PbCH2I) in ether at -50°C under N2; slow warming to room temp.; stirring for 1 h; hydrolysis with H2O;; extn. with CHCl3 two times; drying of the extract over Na2SO4; evapn.; column chromy. of the oily residue (SiO2, benzine/ether (10:1)); recrystn. (benzine, several times); elem. anal.;;
- Guidance literature:
-
With
phenyllithium;
Yield given. Multistep reaction;
1.) ether, benzene, -70 to 0 deg C; 0.5 h, 0 deg C, 2.) ether, benzene, 2 h, r.t.;