Помогите найти методику получения CuBr*Me2S

[OrganicChemist]

Добрый вечер, уважаемые коллеги. Может кто из Вас делал комплекс CuBr*Me₂S и/или знает, где найти методику его получения? Глубоко признателен за советы, ссылки и рекомендации по данному вопросу.

[Vittorio]

H. O. House, C.-Y. Chu, J. M.Wilkins and M. J. Umen, J. Org. Chem.,
1975, 40, 1460–1469.

Preparation of the MezS Complexes of Copper(1) Halides.
A. Me2SCuBr (2).12 To 40.0 g (279 mmol) of pulverized CuBr
(Fisher Scientific) was added 50 ml (42.4 g, 682 mmol) of MeZS
(Eastman, bp 36-38'). The resulting mixture, which warmed during
dissolution, was stirred vigorously and then filtered through a
glass wool plug. The residual solid was stirred with an additional
30 ml (25 g, 409 mmol) of MezS to dissolve the bulk of the remaining
solid and this mixture was filtered. The combined red solutions
were diluted with 200 ml of hexane. The white crystals that separated
were filtered with suction and washed with hexane until the
washings were colorless. The residual solid was dried under nitrogen
to leave 51.6 g (90.h) of the complex 2 as white prisms that dissolved
in an EtzO-MezS mixture to give a colorless solution. For
recrystallization, a solution of 1.02 g of the complex in 5 ml of
MezS was slowly diluted with 20 ml of hexane to give 0.96 g of the
pure complex 2 as colorless prisms, mp 124-129' dec. The complex
2 is essentially insoluble in hexane, EtzO, acetone, CHC13, Cc14,
MeOH, EtOH, and HzO. Although the complex 2 does dissolve in
DMF and in DMSO, the facts that heat is evolved and the resulting
solutions are green colored suggests that the complex has dissociated
and that some oxidation (or disproportionation) to give
Cu(I1) species has occurred. A solution prepared from the complex
2 and DMSO-& exhibited an NMR peak at 6 2.17 (CH3S); a solution
of MezS in the same solvent exhibited a peak at S 2.05. The
complex 2 would dissolve to give a colorless solution in PhH, EtZO,
MeOH, or CHCls when excess MezS was added to the mixture,
suggesting the reversible formation of a more soluble complex such
as (MezS)zCuBr or (MezS)&uBr.
Anal. Calcd for CnHsBrCuS: C, 11.68; H, 2.94; Br, 38.87; S, 15.60.
Found: C, 11.50;H , 2.91;B r, 38.75;S , 15.51.

[Vittorio]

сама статья

и еще одна - из бензилбромида , меди(0) и ДМСО

[Lantanoid]

Добрый вечер, уважаемые коллеги. Может кто из Вас делал комплекс CuBr*Me₂S и/или знает, где найти методику его получения? Глубоко признателен за советы, ссылки и рекомендации по данному вопросу.

ничо страшного в этой реакции нет
думал провоняю (а делали много) - нифига все в порядке и соседи не жаловались, но диметилсульфида надо больше чем в методике - он сильно улетает

[OrganicChemist]

Спасибо, коллеги. Все получилось.