Title compounds \[Et 3 N-CH 2 Cl\] + \[COO-Y-COOH\] - (the la tter is pyridine-2,6- dicarboxyl or dithio (bis-2,2′-benzoyloxy) wer e synthesized by reaction of pyridine-2,6-dicarboxylic aicd or dithio(bis-2,2 ′- ben...Title compounds \[Et 3 N-CH 2 Cl\] + \[COO-Y-COOH\] - (the la tter is pyridine-2,6- dicarboxyl or dithio (bis-2,2′-benzoyloxy) wer e synthesized by reaction of pyridine-2,6-dicarboxylic aicd or dithio(bis-2,2 ′- benzoic aicd) with CH 2 Cl 2 and triethylamine in 1∶1 molar ratio and characterized by elemental analysis, IR and 1 H NMR . Their crystal structures were determined by X-ray single crystal diffractometry, the crystal(Ⅰ) belongs to orthorhombic with a=0 699 43(14) nm, b=1 348 9(3 ) nm, c=1 668 9(3) nm, V= 1 574 5(6) nm 3 , Z=4, D c =1 336 Mg/m 3 , μ=0 259 mm -1 , R 1 =0 033 4, wR 2 =0 080 6, F(000)=672. The crystal(Ⅱ) belongs to triclinic with a=0 788(12) nm, b=1 239(19) nm, c=2 18(3) nm, α= 89 2°, β =89 6°, γ=76 9°, V=2 078(55) nm 3 , Z=4, D c=1 457 Mg/m 3 , μ=0 414 mm -1 , R 1 =0 062 0, wR 2 =0 151 6, F(000)=960.展开更多
The title compounds, C12HIoN307SCI （I） and C15H27NO3S （II）, crystallize in the monoclinic system, space group P21/c with a = 7.3995（1）, b = 27.8489（6）, c = 9.8246（2）/, fl = 131.349（1）, V = 1519.82（5） A3,...The title compounds, C12HIoN307SCI （I） and C15H27NO3S （II）, crystallize in the monoclinic system, space group P21/c with a = 7.3995（1）, b = 27.8489（6）, c = 9.8246（2）/, fl = 131.349（1）, V = 1519.82（5） A3, Z = 4, F（000） = 768, Rint = 0.033 and S = 1.03 for I, and in the orthorhombic system, space group Pbca with a = 8.6227（1）, b = 16.1480（4）, c = 23.8774（6）/, V= 3324.67（12） A3, Z = 8, F（000） = 1312, Rint = 0.024 and S = 1.04 for II. We have devised a convenient procedure for the synthesis of fused organic salts resulting from 1：1 proton-transfer, using an amine and a derivative ofbenzenesulfonic acid. The synthesized salts have a number of applications ranging from their consumption as eco-friendly solvents and catalysts in organic syntheses, to being used as efficient precursors for the production of sulfa drugs. Structures of compounds 3-chloroanilinium 2,4-dinitrobenzenesulfonate （CA-DNBS） and triethylaminium 2,4,6-trimethylbenzenesulfonate （TEA-TMBS） were determined by single-crystal X-ray diffraction studies and infrared spectroscopy.展开更多
文摘Title compounds \[Et 3 N-CH 2 Cl\] + \[COO-Y-COOH\] - (the la tter is pyridine-2,6- dicarboxyl or dithio (bis-2,2′-benzoyloxy) wer e synthesized by reaction of pyridine-2,6-dicarboxylic aicd or dithio(bis-2,2 ′- benzoic aicd) with CH 2 Cl 2 and triethylamine in 1∶1 molar ratio and characterized by elemental analysis, IR and 1 H NMR . Their crystal structures were determined by X-ray single crystal diffractometry, the crystal(Ⅰ) belongs to orthorhombic with a=0 699 43(14) nm, b=1 348 9(3 ) nm, c=1 668 9(3) nm, V= 1 574 5(6) nm 3 , Z=4, D c =1 336 Mg/m 3 , μ=0 259 mm -1 , R 1 =0 033 4, wR 2 =0 080 6, F(000)=672. The crystal(Ⅱ) belongs to triclinic with a=0 788(12) nm, b=1 239(19) nm, c=2 18(3) nm, α= 89 2°, β =89 6°, γ=76 9°, V=2 078(55) nm 3 , Z=4, D c=1 457 Mg/m 3 , μ=0 414 mm -1 , R 1 =0 062 0, wR 2 =0 151 6, F(000)=960.
文摘The title compounds, C12HIoN307SCI （I） and C15H27NO3S （II）, crystallize in the monoclinic system, space group P21/c with a = 7.3995（1）, b = 27.8489（6）, c = 9.8246（2）/, fl = 131.349（1）, V = 1519.82（5） A3, Z = 4, F（000） = 768, Rint = 0.033 and S = 1.03 for I, and in the orthorhombic system, space group Pbca with a = 8.6227（1）, b = 16.1480（4）, c = 23.8774（6）/, V= 3324.67（12） A3, Z = 8, F（000） = 1312, Rint = 0.024 and S = 1.04 for II. We have devised a convenient procedure for the synthesis of fused organic salts resulting from 1：1 proton-transfer, using an amine and a derivative ofbenzenesulfonic acid. The synthesized salts have a number of applications ranging from their consumption as eco-friendly solvents and catalysts in organic syntheses, to being used as efficient precursors for the production of sulfa drugs. Structures of compounds 3-chloroanilinium 2,4-dinitrobenzenesulfonate （CA-DNBS） and triethylaminium 2,4,6-trimethylbenzenesulfonate （TEA-TMBS） were determined by single-crystal X-ray diffraction studies and infrared spectroscopy.
