REACTIONS OF DICHLOROMETHANE WITH CHALCOGENS
1741
5. Garnovskii, A.D., Sadimenko, A.P., Osipov, O.A., and
Tsintsadze, G.V., Zhestko-myagkie vzaimodeistviya v
koordinatsionnoi khimii (Hard–Soft Interactions in the
Coordination Chemistry), Rostov-na-Donu: Rost. Gos.
Univ., 1986.
1.58 g, was added to a solution of 2.38 g of KOH in
10.6 g of hydrazine hydrate, and the mixture was stirred
for 2 h at 80–85°С. In a separate flask, a solution of
tellurium was prepared from 1.07 g of powdered
tellurium, 2.82 g of KOH, and 25.2 g of hydrazine
hydrate under the above conditions. Then the reaction
mixtures were cooled, combined, and, after slow addition
of 1.43 g of dichloromethane and 3-h stirring at 40–43°С,
diluted with water, extracted with dichloromethane, and
dried over MgSO4. The solvent was removed, and the
residue was dried in a vacuum to obtain 1.28 g of a dark
red oily material which, according to GC and GC–MS
data, comprised bis(methylselanyl)methane (Ib), 2,4,6-
triselenaheptane (IIb), bis(methyltellanyl)methane (Ic),
2,6-diselena-4-telluraheptane (Xb), (methylselanyl)
(methyltellanyl)methane (XIb), 2-selena-4,6-ditellura-
heptane (XIII), and dimethyl ditelluride. The mass
spectra of compounds Ib, Ic, and IIb are given above.
Mass spectrum of Xb, m/z (I, % of the total ion current)
(80Se, 130Те): 348 (9.3) [M]+·, 333 (4.8) [M – Me]+, 253
(0.8) [M – MeSe]+, 239 (8.1) [M – MeSeCH2]+, 224
(2.2) [CH2TeSe]+·, 210 (3.1) [SeTe]+·, 159 (1.1)
[MeТeCH2]+, 144 (4.7) [CH2Тe]+·, 130 (1.6) [Тe]+, 109
(45.6) [MeSeCH2]+, 93 (12.8) [CHSe]+, 83 (5.9)
[H3Se]+. Mass spectrum of XIb, m/z (I, % of the total
ion current) (80Se, 130Те): 254 (21.5) [M]+·, 239 (2.4)
[M – Me]+, 224 (2.5) [M – C2H6]+·, 210 (1.6) [TeSe]+·,
159 (2.7) [CH2TeMe]+, 144, 143 (11.3) [CH2Te]+· ,
[CHTe]+, 130 (7.1) [Тe]+, 109 (37.4) [MeSeCH2]+, 93
(10.2) [CHSe]+, 83 (3.3) [H3Se]+. Mass spectrum of
XIII, m/z (I, % of the total ion current) (80Se, 130Те):
398 (5.6) [M]+·, 383 (3.7) [M – Me]+, 289 (12.5) [M –
MeSeCH2]+, 274 (3.8) [CH2Te2]+·, 253 (6.8) [M –
MeTe]+, 238 (1.5) [C2H4SeTe]+·, 224 (0.5) [CH2SeTe]+·,
210 (0.4) [SeTe]+·, 159 (9.8) [MeTeCH2]+, 144 (10.1)
[CH2Te]+·, 131 (6.1) [HTe]+, 109 (29.7) [MeSeCH2]+ ,
94, 93 (6.3) [CH2Se]+·, [CHSe]+, 83 (3.2) [H3Se].
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RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 78 No. 9 2008