Technology Process of ethyldiphenylphosphine-borane
There total 2 articles about ethyldiphenylphosphine-borane which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
With
CeCl3*7H2O; LiAlH4;
In
tetrahydrofuran;
CeCl3*7H2O was stirred in vac. at 140°C for 1 h, maintained at this temp. for 2 h; THF was added under N2; NaBH4 was added; stirring for1 h; phosphine oxide was added (ice bath), followed by LiAlH4 portionwise; stirring at room temp. for 2-15 h; diln. with benzene, pouring in ice/water/HCl; filtration through Celite; org. layer sepn.; extn. of aq. layer with C6H6; combined exts. was dried (Na2SO4) and evapd.; chromy. on silica gel; elem. anal.;
DOI:10.1021/ja00304a061
- Guidance literature:
-
ethylmagnesium bromide; chloro-diphenylphosphine;
In
tetrahydrofuran; diethyl ether;
at 0 - 20 ℃;
for 20h;
Inert atmosphere;
Schlenk technique;
borane-THF;
In
tetrahydrofuran; diethyl ether;
at 20 ℃;
for 3h;
Inert atmosphere;
Schlenk technique;
DOI:10.1021/acs.joc.7b01767
- Guidance literature:
-
ethyldiphenylphosphine-borane;
With
(2-methylpropyl)lithium;
In
tetrahydrofuran;
at -78 ℃;
for 1h;
Inert atmosphere;
Schlenk technique;
(3-chloropropyl)diphenylphosphine-borane;
In
tetrahydrofuran;
at -78 - 20 ℃;
for 2h;
Inert atmosphere;
Schlenk technique;
DOI:10.1021/acs.joc.7b01767