1,3,5,7,2,4,6,8-四硫杂四氮杂环辛四烯合成路线 （共 142 条）
反应条件
silver(I) in ammonia
removal of S(2-) by AgI (formation of Ag2S); filtration; evapn. and heating filtrate (2h/100°C);; evapn. (over H2SO4); extraction (CS2); evapn.;;
参考文献
Ruff, O.; Geisel, E.
Ber., 1905 , vol. 38, p. 2659 - 2667
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Gmelin Handbook: S: MVol.B3, 4, page 1537 - 1540
反应条件
ammonia in benzene
passing ammonia through soln. of S2Cl2 in benzene, addn. of water; according to M. Villena-Blanco, Jolly, W. L., Inorg. Synth., 1967(9), 98; filtration, recrystn. (ethyl acetate), sublimation (vac.);
参考文献
Spitsyn, V. I.; Kolli, I. D.; Orlova, E. M.
Russian Journal of Inorganic Chemistry (Translation of Zhurnal Neorganicheskoi Khimii), 1986 , vol. 31, p. 163 - 166
Zhurnal Neorganicheskoi Khimii, 1986 , vol. 31, p. 291 - 295
反应条件
in neat (no solvent)
decompn. on heating;;
参考文献
Schlossnagel, F.
Z. Anorg. Chem., 1953 , vol. 271, p. 226 - 228
反应条件
Zn in methanol
to methanolic suspension Zn dust is added under heavy shaking (in coldness); the leek green liquid turns dark red; (reaction should be stopped in time to avoid decompn. of S5N2 by Zn);; filtration; evapn. of filtrate;;
参考文献
Muthmann, W.; Clever, A.
Z. Anorg. Chem., 1897 , vol. 13, p. 200 - 208
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Gmelin Handbook: S: MVol.B3, 1, page 1131 - 1533
反应条件
in water
cold (-15°C) aq. HBF4 was added to compound, shaked briefly at room temp. in an ultrasonic bath, left overnight at -15°C;; filtered, solid was washed with cold Et2O, extd. with pentane for 24 h; extd with MeCN for 30 min (soluble product); elem. anal.;;
参考文献
Banister, Arthur J.; Hauptman, Zdenek V.; Kendrick, Aidan G.; Small, Ronald W. H.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1987 , p. 915 - 924
反应条件
in dichloromethane
byproducts: (CH3)3SiCl, N2; a soln. of Si compd. added to a suspn. of TeCl4 at -80°C, stirredovernight, allowed to warm to room temp.; sepd., addnl. crystd. at room temp.;
参考文献
Konu, Jari; Ahlgren, Markku; Aucott, Stephen M.; Chivers, Tristram; Dale, Sophie H.; Elsegood, Mark R. J.; Holmes, Kathryn E.; James, Sarah L. M.; Kelly, Paul F.; Laitinen, Risto S.
Inorganic Chemistry, 2005 , vol. 44, # 14 p. 4992 - 5000
反应条件
SCl2 in not given
reaction of sulfur chloride(s) with ammonia;; sepn. by mixture (water/not miscible organic solvent e.g. CCl4); contaminated by traces of sulfur;;
参考文献
Gmelin Handbook: S: MVol.B3, 5, page 1540 - 1543
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Imperial Chemical Industries of Australia and New Zealand Ltd.
Patent: AU115492 , 1942 ;
C. I, 1946 , p. 776
反应条件
Zn in tetrahydrofuran
stirring at -5°C for 60 h under an atmosphere of dry N2; the solvent was pumped off at -15°C to dryness, reaction products were allowed to warm up to room temp., pumping for 6 h to sublime the product, repeated vac. sublimation;
参考文献
Small, Ronald W. H.; Banister, Arthur J.; Hauptman, Zdenek V.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1981 , p. 2188 - 2191
反应条件
in neat (no solvent)
heating under reflux (4 h), cooling; filtration of polymeric HNCS, further flash chromy. (SiO2, CH2Cl2 (30-40percent) in light petroleum);
参考文献
Dunn, Peter J.; Morris, Janet L.; Rees, Charles W.
Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1988 , p. 1745 - 1748
反应条件
sodium acetate in water
hydrolysis at 0°C; 15 min vigorous shaking in ice cold aq. sodium acetate soln.;; filtration; removal of S4N4 (washing twice/pH 6/aq. acetic acid/ice cold); digesting (twice/ice cold benzene); extraction (CS2/cooled by NaCl-ice/12-15 times/not longer than 1h); washing of ppt. (abs. ether/ice cold/fast); drying (high vac./H2SO4/P2O5);;
参考文献
Meuwsen, A.; Jakob, O.
Z. Anorg. Chem., 1950 , vol. 263, p. 200 - 212
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Gmelin Handbook: S: MVol.B3, 22, page 1575 - 1577
