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Purification of Laboratory Chemicals, 8th Edition by W.L.F. Armarego

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The nitrosate, C15H24N2O4, [-C(NO)—C(ONO2)-] prepared from amyl nitrite and AcOH, then HNO3-AcOH, crystallises from *C6H6, and has m 161° to m 165° depending on heating rate [reported also: 163°]. The nitrosite, C15H24N2O3, [-C(NO)—C(ONO)-] separates as blue crystals when equal volumes of α-humulene and light petroleum are shaken with concentrated aqueous NaNO2 with cooling, followed by slow addition of glacial acetic acid (volume equal to humulene used) with shaking. The organic green-blue layer is separated, and the blue crystals of the nitrosite are collected and crystallised from EtOH to give blue needles of the dinitrosite compound (dimer ?) with m 120-121°. Boiling a solution of the blue nitrosite in EtOH for several hours slowly caused ...

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