Technology Process of {closo-1-(CH3)-8-(C6H5)-1,8-C2B9H9
There total 1 articles about {closo-1-(CH3)-8-(C6H5)-1,8-C2B9H9 which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
polyphosphoric acid;
In
toluene;
under an dry nitrogen or argon; suspn. was refluxed for 3 h and cooled to ambient temp., and the yellow organic layer was cannulated from the reaction flask; repeated washings of the polyphosphoric acid using hot toluene were essential; the toluene from the collected organic fractions were distilled under N2 until a head temp. of 114°C was attained; the remaining oil was purified by vac. sublimation (75°C); elem. anal.;
DOI:10.1021/om00120a004
- Guidance literature:
-
With
triethylamine; NaBH4; {(CH3)3NH}Cl;
In
monoethylene glycol diethyl ether; water;
byproducts: B2H6; a soln. of closo-carborane in diethoxyethane was added dropwise to the rapidly stirred borohydride suspn.; the B2H6 was vented from the top of the reflux condenser under a flow of N2 into a gas scrubber contg. triethylamine in heptane, reflux for 2 h; concn. of the filtered soln. in vac. and addn. of a satd. aq. soln. of ((CH3)3NH)Cl; extn. with CH2Cl2, recrystn. from CH2Cl2/heptane and acetonitrile/heptane; elem. anal.;
DOI:10.1021/om00120a004