PhCH2)3Sn·(O2CC5H4N)·(H2O)]n was synthesized by the reaction of 4-pyridine car-boxylic acid with the tribenzyltin o xide and was characterized by IR,1 H NMR and MS.Its crystal structure was determined by X-r...PhCH2)3Sn·(O2CC5H4N)·(H2O)]n was synthesized by the reaction of 4-pyridine car-boxylic acid with the tribenzyltin o xide and was characterized by IR,1 H NMR and MS.Its crystal structure was determined by X-ray single crystal diffraction.The crystal belongs to monoclinic.The space group P21 /c with unit cell parameters a=1.2241(8)nm,b=0.9660(6)nm,c=2.3708(15)nm,β=102.722(12)°,V=2.734(3)nm3,Z =4,Dc=1.298g·cm-3 .In crystal,the tin atom rendered five-coordinate in a trigo nal bipyramidal structure which is b ridged by 4-pyridine carboxy-late into one-dimensional chain polymers.展开更多
The title compound (C22H18N2O3) has been synthesized by the reaction of 3,4- dimethoxybenzaldehyde, malononitrile and 1-naphthol in ethanol in the presence of piperidine, and its structure was characterized by element...The title compound (C22H18N2O3) has been synthesized by the reaction of 3,4- dimethoxybenzaldehyde, malononitrile and 1-naphthol in ethanol in the presence of piperidine, and its structure was characterized by elemental analysis, IR, 1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group C2/c with a = 24.221(6), b = 9.016(2), c = 17.003(5) ? b = 93.16(1), V = 3707(2) ?, Mr = 358.38, Z = 8, Dc = 1.284 g/cm3, m(MoKa) = 0.087 mm-1, F(000) = 1504, the final R = 0.0432 and wR = 0.1085. X-ray analysis reveals that the atoms of C(1), C(2), C(3), C(4), C(5) and O(1) form a boat-form six-membered ring in which the C(1)C(2) (1.349(3) ? is a C=C double bond.展开更多
以硫脲和氯乙酸为原料,在无溶剂和350 W微波辐射4 m in条件下,缩合生成中间体2,4-噻唑烷二酮(Ⅰ)产率91.5%;随后在无溶剂和400 W微波辐射5 m in条件下,通过V ilsm e ier甲酰化反应,生成中间体4-氯-5-甲酰基噻唑-2(3H)-酮(Ⅱ),产率86.7%...以硫脲和氯乙酸为原料,在无溶剂和350 W微波辐射4 m in条件下,缩合生成中间体2,4-噻唑烷二酮(Ⅰ)产率91.5%;随后在无溶剂和400 W微波辐射5 m in条件下,通过V ilsm e ier甲酰化反应,生成中间体4-氯-5-甲酰基噻唑-2(3H)-酮(Ⅱ),产率86.7%;最后以正丙醇为溶剂,450 W微波辐射7 m in条件下,成环得到5-氨基-噻唑[4,5-d]嘧啶-2(3H)-酮(Ⅲ),产率80.5%。反应总产率为63.9%。合成产物与中间体的结构经1HNMR,MS和元素分析确认。展开更多
A simple and practical route is described for the synthesis of 2-efhoxy-（4H）-3,1 -benzoxazine-4-ones using the coupling reaction of anthranilic acid derivatives with diethyl dicarbonate following with fast cyclizati...A simple and practical route is described for the synthesis of 2-efhoxy-（4H）-3,1 -benzoxazine-4-ones using the coupling reaction of anthranilic acid derivatives with diethyl dicarbonate following with fast cyclization of the carbamate adduct with a dehydrocyclization agent such as cyanuric chloride and N,N′-dicyclohexylcarbodiimide in PEG at room temperature.High yields of the products obtained under mild reaction conditions with simple work-up of the reaction mixture.展开更多
文摘PhCH2)3Sn·(O2CC5H4N)·(H2O)]n was synthesized by the reaction of 4-pyridine car-boxylic acid with the tribenzyltin o xide and was characterized by IR,1 H NMR and MS.Its crystal structure was determined by X-ray single crystal diffraction.The crystal belongs to monoclinic.The space group P21 /c with unit cell parameters a=1.2241(8)nm,b=0.9660(6)nm,c=2.3708(15)nm,β=102.722(12)°,V=2.734(3)nm3,Z =4,Dc=1.298g·cm-3 .In crystal,the tin atom rendered five-coordinate in a trigo nal bipyramidal structure which is b ridged by 4-pyridine carboxy-late into one-dimensional chain polymers.
文摘The title compound (C22H18N2O3) has been synthesized by the reaction of 3,4- dimethoxybenzaldehyde, malononitrile and 1-naphthol in ethanol in the presence of piperidine, and its structure was characterized by elemental analysis, IR, 1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group C2/c with a = 24.221(6), b = 9.016(2), c = 17.003(5) ? b = 93.16(1), V = 3707(2) ?, Mr = 358.38, Z = 8, Dc = 1.284 g/cm3, m(MoKa) = 0.087 mm-1, F(000) = 1504, the final R = 0.0432 and wR = 0.1085. X-ray analysis reveals that the atoms of C(1), C(2), C(3), C(4), C(5) and O(1) form a boat-form six-membered ring in which the C(1)C(2) (1.349(3) ? is a C=C double bond.
文摘以硫脲和氯乙酸为原料,在无溶剂和350 W微波辐射4 m in条件下,缩合生成中间体2,4-噻唑烷二酮(Ⅰ)产率91.5%;随后在无溶剂和400 W微波辐射5 m in条件下,通过V ilsm e ier甲酰化反应,生成中间体4-氯-5-甲酰基噻唑-2(3H)-酮(Ⅱ),产率86.7%;最后以正丙醇为溶剂,450 W微波辐射7 m in条件下,成环得到5-氨基-噻唑[4,5-d]嘧啶-2(3H)-酮(Ⅲ),产率80.5%。反应总产率为63.9%。合成产物与中间体的结构经1HNMR,MS和元素分析确认。
基金the University of Kurdistan Research Council for the partial support of this work
文摘A simple and practical route is described for the synthesis of 2-efhoxy-（4H）-3,1 -benzoxazine-4-ones using the coupling reaction of anthranilic acid derivatives with diethyl dicarbonate following with fast cyclization of the carbamate adduct with a dehydrocyclization agent such as cyanuric chloride and N,N′-dicyclohexylcarbodiimide in PEG at room temperature.High yields of the products obtained under mild reaction conditions with simple work-up of the reaction mixture.
