sulfur

in 1,4-dioxane; water ligand refluxed with P2S5 for 10 h, filtered while hot, aq. soln. of NiCl2 added (10:15:4.9 molar ratio), refluxed for 2-4 h; crystd. on cooling, crystd., filtered off, washed (dioxane, H2O, EtOH, ether), dried, recrystd. (DCM), elem. anal.;

in 1,4-dioxane; water PhCOCHOHPh and P4S10 reacted in dioxane under reflux for 2 h, NiCl2*6H2O added, mixture reacted in dioxane/water under reflux; elem. anal.;

in 1,4-dioxane; water Ar, Br compds. heated in dioxane with S compd. (2 equiv.) at 110°C for 5-6 h, filtered, an aq. soln. of Ni salt added, refluxed for 2 h; filtered, washed (methanol, water) recrystd. (CH2Cl2/methanol); elem. anal.;

NaOMe; aq. HCl in methanol (N2); MeOH soln. of NaOMe added to organic ligands in MeOH; mixt. stirred for 30 min; NiCl2*6H2O in MeOH added dropwise within 15 min; stirred for 1 h at room temp.; aq. HCl added; mixt. stirred in air overnight; washed with water and MeOH; dried in air; extracted with CS2; chromatographed on silica gel using CS2 as eluent; elem. anal.;

NaOMe; aq. HCl in methanol (N2); MeOH soln. of NaOMe added to organic ligands in MeOH; mixt. stirred for 30 min; NiCl2*6H2O in MeOH added dropwise within 15 min; stirred for 1 h at room temp.; aq. HCl added; mixt. stirred in air overnight; washed with water and MeOH; dried in air; extracted with CS2; chromatographed on silica gel using CS2 as eluent; elem. anal.;

in benzene byproducts: norbornadien; Irradiation (UV/VIS);

in chloroform-d1 byproducts: 7-acetoxynorbornadiene; Irradiation (UV/VIS); CDCl3, ambient light, 35 h;

in benzene 2.5 h; Heating;

in benzene Ni-complex and org. ligand dissoln., mixt. refluxing under Ar for 2.5 h, org. ligand removal (red. pressure); column chromy. (silica gel, n-hexane/dichloromethane), thin layer chromy. (plate, Kieselgel, n-hexane/dichloromethane); elem. anal.;