MARTINJ. SCHICK, PAULDOTYAND BRUNOH. ZIMM
530
Vol. 72
TABLE I1 hll. Ma"
Solvent
1 2 3 4 5c 6 7
Solvent, ml.
10 Alcohol 50 10 Alc.-H20 50-55 Ether 30 20 20 35 Ether 16 50 Benzene . 50 hf2 50 M2 8" 65 . hI2 &I? .. 9 50 * Mz = hexamethyldisiloxane. KOH hydrolyzed t o yield trimethylsilanol.
Base
G. of base
2.13 IU4,320,24A KOH KOH 2.41 %UU KOHb 10 "00 KOH 4 19(J KOH > 190 KOH 5 190 KOH* 5.5 185 NaOH 5 150 XaOH 3 190 not fused. Platinum thimble used
of metallic sodium with trimethylsilanol. Hydrolysis of a sample of the solid from reaction 9 was carried out with cold water in a small test-tube t o yield hexamethyldisiloxane. The infrared spectrogram of this liquid was identical with that obtained from a pure sample of, hexamethyldisiloxane. The refractive index a t 20 was 1.3772 (reported in the literature, 1.37740 and 1.37723).
Summary The action of sodium and potassium hydroxides (6) Burkbard, Rochow, Booth and Hartt, Chcm. Reus., 41, 127 11947).
[CONTRIBUTION FROM
THE
Ream. temp, O C
Time, hr.
Resid. At temp. P(p.s.i.) OC.
% Na or IC
680 5 22.2 93 655 6 24.2 1U6 11 160 15 33.4 73.5 110 12 36.5 200 24 30.8 118 61.5 290 24 35.7 440 24 .. d 13
