My PhD dissertation - Institut Fresnel
My PhD dissertation - Institut Fresnel
My PhD dissertation - Institut Fresnel
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83<br />
13 C NMR: δ = 43.8 (d, J = 14 Hz), 30.7 (d, J = 13 Hz), 28.8 (d, J = 15 Hz), 25.3<br />
(d, J = 12 Hz), 16.4 (d, J = 3 Hz), 14.9 ppm.<br />
31 P NMR: δ = 56.9 ppm.<br />
Diethyl-N,N-diethylaminophosphine (24c): Prepared following the procedure described by<br />
K. Issleib and W. Seidel [147] ; colorless liquid; b.p. 44 - 47 °C/12 Torr (ref. [147] b.p. 181°C);<br />
yield: 13.0 g (81%).<br />
1 H NMR: δ = 2.93 (symm. m, 4 H), 1.5 (m, 2 H), 1.2 (m, 2 H), 1.02 (symm. m,<br />
12 H) ppm.<br />
13 C NMR: δ = 42.8 (d, J = 13.3 Hz), 22.2 (d, J = 10.9 Hz), 15.5 (d, J = 2.8 Hz),<br />
9.7 (d, J = 16.1 Hz) ppm.<br />
31 P NMR: δ = 65.2 ppm.<br />
Dimethyl-N,N-diethylaminophosphine (24d): Prepared by addition of methyllithium in<br />
diethyl ether (0.14 L); colorless liquid; b.p. 46 - 49 °C/59 Torr (ref. [149] b.p. 48 °C/35 Torr);<br />
20 n D = 1,4492 (ref.<br />
[149] n 20 = 1.4472); yield: 6.51 g (49%).<br />
D<br />
1 H NMR: δ = 2.80 (qd, J = 9.6, 7.0 Hz, 4 H), 1.01 (d, J = 6.0 Hz, 6 H), 0.94 (t,<br />
J = 7.0 Hz, 6 H) ppm.<br />
13 C NMR: δ = 22.5 (d, J = 11.9 Hz), 16.1 (d, J = 2.6 Hz), 9.9 (d, J = 16.4 Hz)<br />
ppm.<br />
31 P NMR: δ = 34.7 ppm.<br />
3.1.2 Dialkylchlorophosphines<br />
Di-tert-butylchlorophosphine (25a): A 5.8 M hydrogen chloride solution in diethyl ether<br />
(0.10 L) was slowly added to a solution of di-tert-butyl-N,N-diethylaminophosphine (24a;<br />
43 g, 0.20 mol) in diethyl ether (0.10 L) at -75 °C. The salts were removed by filtration under<br />
inert atmosphere and the mother liquors transferred via a canula to the usual distillation