2-Oxo-3R,4S,5S,6S-tetraethoxyazepane was conveniently synthesized from D-glucono-1, 5-1actone with a yield of 10% overall. The key step of synthetic route-reductive 1,6-cyclization was completed efficiently by using P...2-Oxo-3R,4S,5S,6S-tetraethoxyazepane was conveniently synthesized from D-glucono-1, 5-1actone with a yield of 10% overall. The key step of synthetic route-reductive 1,6-cyclization was completed efficiently by using Ph3P to give the expected lactam.展开更多
A photocatalytic tandem cyclization of o-alkenylbenzaldehydes using pyridinium salts as the amination reagent is described.A variety of valuable seven-membered nitrogenous heterocyclic skeletons are prepared in modest...A photocatalytic tandem cyclization of o-alkenylbenzaldehydes using pyridinium salts as the amination reagent is described.A variety of valuable seven-membered nitrogenous heterocyclic skeletons are prepared in modest to excellent yields in concise one-step.This transformation features mild reaction conditions and exceptional functional group tolerance.In addition,combining control experiments and density functional theory(DFT)calculations on the mechanism can explain the reaction selectivity.展开更多
The title compound （2-iodo-5-nitrophenyl）-[1-（1-methylazepan-3-yl）-lH-indol-3- yl]methanone （C22H22IN303, Mr- 503.07 ） was synthesized by the reaction of 3-（2-iodo-5- nitrobenzoyl）indole with 2-chloromethyl-1-...The title compound （2-iodo-5-nitrophenyl）-[1-（1-methylazepan-3-yl）-lH-indol-3- yl]methanone （C22H22IN303, Mr- 503.07 ） was synthesized by the reaction of 3-（2-iodo-5- nitrobenzoyl）indole with 2-chloromethyl-1-methylpiperidine. Its chemical structure was determined by 1H NMR, 13C NMR, DEPT, COSY, HMQC, HMBC, HRMS and X-ray single-crystal diffraction. The crystal belongs to the triclmic system, space group P1 with a = 9.153（4）, b = 10.409（3）, c = 11.882（4） A, a = 71.84（3）, β = 78.67（3）, ）, = 75.49（3）°, V = 1032.7（6） A3, Z = 2, Dc= 1.619 g/era3, = 1.579 mm-1, F（000） = 504, R = 0.0270 and wR = 0.0498 for 3634 observed reflections with I 〉 20（/）. X-ray analysis shows that the indole ring forms a dihedral angle of 84.57（12）° with the iodobenzene ring and the azepane ring adopts a twisted chair conformation. Weak C-H...O hydrogen bonding contributes to the stability and packing of the structure.展开更多
基金the Graduate Education Innovation Foundation of Nanjing University of Science & Technology (No.200705).
文摘2-Oxo-3R,4S,5S,6S-tetraethoxyazepane was conveniently synthesized from D-glucono-1, 5-1actone with a yield of 10% overall. The key step of synthetic route-reductive 1,6-cyclization was completed efficiently by using Ph3P to give the expected lactam.
基金the National Natural Science Foundation of China(21632003,21871116)the Key Program of Gansu Province(17ZD2GC011)the‘‘111’’Program from the MOE of China。
文摘A photocatalytic tandem cyclization of o-alkenylbenzaldehydes using pyridinium salts as the amination reagent is described.A variety of valuable seven-membered nitrogenous heterocyclic skeletons are prepared in modest to excellent yields in concise one-step.This transformation features mild reaction conditions and exceptional functional group tolerance.In addition,combining control experiments and density functional theory(DFT)calculations on the mechanism can explain the reaction selectivity.
基金Supported by Hunan Provincial Key Laboratory of Materials Protection for Electric Power and Transportation (2013CL09, 21275022)Changsha University of Science & Technology,National Natural Science Foundation of China (21202010)Natural Science Foundation of Hunan Province (12JJ4021)
文摘The title compound （2-iodo-5-nitrophenyl）-[1-（1-methylazepan-3-yl）-lH-indol-3- yl]methanone （C22H22IN303, Mr- 503.07 ） was synthesized by the reaction of 3-（2-iodo-5- nitrobenzoyl）indole with 2-chloromethyl-1-methylpiperidine. Its chemical structure was determined by 1H NMR, 13C NMR, DEPT, COSY, HMQC, HMBC, HRMS and X-ray single-crystal diffraction. The crystal belongs to the triclmic system, space group P1 with a = 9.153（4）, b = 10.409（3）, c = 11.882（4） A, a = 71.84（3）, β = 78.67（3）, ）, = 75.49（3）°, V = 1032.7（6） A3, Z = 2, Dc= 1.619 g/era3, = 1.579 mm-1, F（000） = 504, R = 0.0270 and wR = 0.0498 for 3634 observed reflections with I 〉 20（/）. X-ray analysis shows that the indole ring forms a dihedral angle of 84.57（12）° with the iodobenzene ring and the azepane ring adopts a twisted chair conformation. Weak C-H...O hydrogen bonding contributes to the stability and packing of the structure.
