Plate, A F’s team published research in Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya in 1956 | 20744-39-2

Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya published new progress about Bond. 20744-39-2 belongs to class pyridazine, and the molecular formula is C4H5N3, SDS of cas: 20744-39-2.

Plate, A. F.; Belikova, N. A.; Egorov, Yu. P. published the artcile< Reaction of five- and six-membered silicohydrocarbons with an atom of silicon in the ring with concentrated sulfuric acid>, SDS of cas: 20744-39-2, the main research area is .

Concentrated H2SO4 caused a rupture of the C-Si bond in cyclic 5-6 membered silanes; the 5-membered ring was somewhat more stable. The method of West (C.A. 49, 14767b) gave 26.6% Si[(CH2)4]2, b750 173-4°, nD20 1.4863, d20 0.9043, m. -52°. This (4.3 g.) shaken 6 hrs. at room temperature with 11.7 g. concentrated H2SO4 gave 4 g. [Bu(CH2)4Si]2O, 90%, b751 293.5-94°, nD20 1.4670, d20 0.9125. Similarly [Et(CH2)4Si]2O in 10 hrs. gave 60% sym-tetraethyltetrabutylcyclotetrasiloxane, b10 194-6°, nD20 1.4422, d20 0.9286. To the Grignard reagent from 37 g. Mg and 161 g. (CH2)5Br2 was added at once at 5° 90 g. Me2SiCl2 in 1 l. Et2O and, after refluxing 15 hrs. and treatment with H2O, there was obtained after distillation and chromatographic purification on silica, 26.7% Me2Si(CH2)5, b740 131.2-1.3°, nD20 1.4428, d20 0.8111, Raman spectrum (cm.-1) 105(15), 146(30), 203(70), 238(18), 253(15), 334(25), 371(10), 482(10), 585(200), 632(5), 663(2), 694(15), 724(15), 741(5), 794(40), 833(3), 908(30), 950(3), 990(8), 1006(40), 1037(2), 1080(12), 1098(10), 1134(15), 1180(19), 1193(15), 1251(15), 1268(12), 1291(15), 1333(7), 1408(15), 1445(25), 1460(10), 2846(75), 2874(20), 2900(125), 2928(15), 2965(50). This shaken with H2SO4 13.5 hrs. gave some CH4 and 85% mixed disiloxanes (I), presumably sym-diamyltetramethyldisiloxane, sym-dimethylbispentamethylenedisiloxane, and AmMe2SiOSiMe(CH2)5. Presumably the cleavage of the rings took place through formation of intermediate sulfate ester of the resulting silanol, and with a 6-membered ring it could take place in 2 possible directions as shown. Si[(CH2)4]2 had Raman spectrum: 242(15), 305(60), 591(25), 618(55), 668(15), 726(10), 757(5), 782(5), 854(60), 946(30), 1026(35), 1068 (12), 1156(20), 1200(7), 1254(25), 1340(5), 1414(25), 1457(35), 2854(120), 2870(35). 2895(135), 2945(275). sym-Tetramethyldiamyldisiloxane has Raman spectrum: 170 (2) 200(4), 479(1), 540(6), 652(5), 682(5), 705(3), 763(1), 767(1), 838(0), 895(4), 922(1), 956(4), 1026(3), 1070(3), 1102(43), 1135(4), 1186(6), 1245(4), 1262(1), 1304(6), 1336(1), 1380(1), 1410(5), 1443(7), 1456(5), 2858(5), 2882(5), 2904(10), 2965(10). I, b. 245-52°, nD20 1.4430, d20 0.8681, was presumed to have the above indicated composition on the basis of elemental analysis and Raman spectrum.

Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya published new progress about Bond. 20744-39-2 belongs to class pyridazine, and the molecular formula is C4H5N3, SDS of cas: 20744-39-2.

Referemce:
Pyridazine – Wikipedia,
Pyridazine | C4H4N2 – PubChem