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Papers by Anestis Logothetis
J Org Chem, 1966
9,lO-Dichloro-9,1O-bis(difluoramino)-9,1O-dihydroanthracene (Ilc and IIc).-In a 240-ml tube conta... more 9,lO-Dichloro-9,1O-bis(difluoramino)-9,1O-dihydroanthracene (Ilc and IIc).-In a 240-ml tube containing 30 g (0.12 mole) of 9,lO-dichloroanthracene and 60 g of benzene was condensed 14.0 g (0.135 mole) of NZF4, and the tube was sealed and shaken a t 71' for 1 hr. The benzene-insoluble solid was unreacted 9,lOdichloroanthracene and was removed by filtration. The benzene solution was evapnr-ted in vacuo to give 23.0 g (54%) of 9,lOdichloro-9,10-bis(difluoramino)anthracene as a mixture of cis and trans isomers. It was carefully recrystallized from petroleum ether (40-6O0)-benzene with the minimum of heating to give 20 g of white, cubic crystals: mp 120-125' dec; infrared maxima (Nujol), 10.17 (m), 10.57 (s), 11.32 (s), 11.57 (sh) (m), 11.72 (sh) (m) (NF2), and 13.40 (s) p (aromatic); ultraviolet absorption (EtOH), 273 mp (e 1600), 280 (1490), 298 (157), 309 (loo), 332 and (42.5); F19 nmr (nitrobenzene),-6175 cps and-6075 cps (NF2) in about 2: 1 ratio.
J Org Chem, 1966
9,lO-Dichloro-9,1O-bis(difluoramino)-9,1O-dihydroanthracene (Ilc and IIc).-In a 240-ml tube conta... more 9,lO-Dichloro-9,1O-bis(difluoramino)-9,1O-dihydroanthracene (Ilc and IIc).-In a 240-ml tube containing 30 g (0.12 mole) of 9,lO-dichloroanthracene and 60 g of benzene was condensed 14.0 g (0.135 mole) of NZF4, and the tube was sealed and shaken a t 71' for 1 hr. The benzene-insoluble solid was unreacted 9,lOdichloroanthracene and was removed by filtration. The benzene solution was evapnr-ted in vacuo to give 23.0 g (54%) of 9,lOdichloro-9,10-bis(difluoramino)anthracene as a mixture of cis and trans isomers. It was carefully recrystallized from petroleum ether (40-6O0)-benzene with the minimum of heating to give 20 g of white, cubic crystals: mp 120-125' dec; infrared maxima (Nujol), 10.17 (m), 10.57 (s), 11.32 (s), 11.57 (sh) (m), 11.72 (sh) (m) (NF2), and 13.40 (s) p (aromatic); ultraviolet absorption (EtOH), 273 mp (e 1600), 280 (1490), 298 (157), 309 (loo), 332 and (42.5); F19 nmr (nitrobenzene),-6175 cps and-6075 cps (NF2) in about 2: 1 ratio.