New P-S-N containing ring systems. Reaction of 2,4-(naphthalene-1,8-diyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide with methylbis(trimethylsilyl)amine
P. Kilian et al., New P-S-N containing ring systems. Reaction of 2,4-(naphthalene-1,8-diyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide with methylbis(trimethylsilyl)amine, J CHEM S DA, (13), 1999, pp. 2231-2236
Citations number
16
Categorie Soggetti
Inorganic & Nuclear Chemistry
Journal title
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS
From the reaction of 2,4-(naphthalene-1,8-diyl)-1,3,2,4-dithiadiphosphetane
2,4-disulfide 1 with methylbis(trimethylsilyl)amine 2 in dichloromethane a
product of the P2S2 ring cleavage, (C10H6)P(S)(SSiMe3)(mu-S)P(S)(NMeSiMe3)
3, was isolated, existing in an equilibrium between two diastereomeric for
ms in solution. Compound 3 was also obtained when toluene was used as a sol
vent. Its subsequent reaction with pyridine (py) led to the desilylated ion
ic product [Hpy(+)][(C10H6)P(S)(NHMe)(mu-S)PS2-] 4, which reacts with tetra
phenylphosphonium chloride to give [PPh4+][(C10H6)P(S)(NHMe)(mu-S)PS2-] 5.
When acetonitrile was used as a solvent a cage compound 2,6-(naphthalene-1,
8-diyl)-3,4-dimethyl-1,3,5,2 lambda(5),6 lambda(5)-thiadiazadiphosphinine 2
,6-disulfide 6 containing a six-membered CN2P2S heterocycle was obtained. T
he new compounds were studied spectroscopically (1- and 2-D high resolution
NMR, IR, MS) and in the cases of 3, 5 and 6 by X-ray crystallography.