The synthesis of an new photochromical compound,1,3,3 trimethyl 6′ (1 piperidinyl) spiro[2h indole 2,3′ [3H]pyridobenzoxazine (SP3),and an improved way for the synthesis of 6 hydroxyquinoline were descrided.The abso...The synthesis of an new photochromical compound,1,3,3 trimethyl 6′ (1 piperidinyl) spiro[2h indole 2,3′ [3H]pyridobenzoxazine (SP3),and an improved way for the synthesis of 6 hydroxyquinoline were descrided.The absorption spectrum of the colored metastable form SP3 shows prominent absorption peak at 560nm at 60℃?展开更多
Reaction of 2,4-di-Eert-butyl-phenol,ethylenediamine and formaldehyde (37% solution in water)in 2:1:5molar ratio in methanol afforded the 1,2-bis[3-(6,8-di-tert-butyl-3,4-dihydro-2[H]-1,3-benzoxazine)-yl]ethane in...Reaction of 2,4-di-Eert-butyl-phenol,ethylenediamine and formaldehyde (37% solution in water)in 2:1:5molar ratio in methanol afforded the 1,2-bis[3-(6,8-di-tert-butyl-3,4-dihydro-2[H]-1,3-benzoxazine)-yl]ethane in high yields.This compound was fully characterized by elemental analysis,1H NMR,MS,and IR spectroscopies.The crystal structure of the title compound was determined by X-ray diffraction method.It crystallizes in triclinic,space group P(1),a=0.5727(2),b=0.9268(3),c=1.4666(4)nm,a=88.12(1)°,β=88.54(1)°,γ=80.82(1)°,V=0.7679(4)nm3,Z=1,DC=1.126Mg·m-3,F(000)=286,μ(MoKα)=0.69cm-1,R=0.048,wR=0.140.This compound had a centrosymmetrical structure.展开更多
Benzoxazinone usually exists in many kinds of plants.It is applied in prepharmacy synthesis,and bioactivity studies,and has been prepared from O-aminophenol and chrol-with alkine and solvent by refluxing for a long ti...Benzoxazinone usually exists in many kinds of plants.It is applied in prepharmacy synthesis,and bioactivity studies,and has been prepared from O-aminophenol and chrol-with alkine and solvent by refluxing for a long time.In this work,2,2’-diphenyl-1,4-benzoxazin-3(4H)-one was solvent-free synthesized under microwave irradiation.The configuration and conformation of the product were determined by 1H NMR,IR,MS,elementary analysis and X-ray crystal analysis.The results of X-ray crystal analysis show that the compound crystallizes in a triclinic system,space group %P%1,cell parameter %a%=0.840 7(1)nm,%b%=0.845 1(1)nm,%c%=2.254 1(3)nm,%α%=96.111(3)°,%β%=97.196(3)°,%γ%=90.229(3)°,%V%= 1^579 6(4)nm3,%Z%=4,%D%c =1.267 Mg/m3,%F%(000)= 632.0,%μ%= 0.08 mm-1.In the compound,oxazinone ring is shown chair conformation,two benzene rings is placed in two sides of oxazinone ring distortedly.In crystal state,a centrosymmetric dimmer is formed %via% hydrogen bonds generated from amides of two near molecules.The benzene rings in a same chemical environment are paralleled by a distance of 0.260 9 nm.It displays aromatic π-π stacking interactions.展开更多
文摘The synthesis of an new photochromical compound,1,3,3 trimethyl 6′ (1 piperidinyl) spiro[2h indole 2,3′ [3H]pyridobenzoxazine (SP3),and an improved way for the synthesis of 6 hydroxyquinoline were descrided.The absorption spectrum of the colored metastable form SP3 shows prominent absorption peak at 560nm at 60℃?
文摘Reaction of 2,4-di-Eert-butyl-phenol,ethylenediamine and formaldehyde (37% solution in water)in 2:1:5molar ratio in methanol afforded the 1,2-bis[3-(6,8-di-tert-butyl-3,4-dihydro-2[H]-1,3-benzoxazine)-yl]ethane in high yields.This compound was fully characterized by elemental analysis,1H NMR,MS,and IR spectroscopies.The crystal structure of the title compound was determined by X-ray diffraction method.It crystallizes in triclinic,space group P(1),a=0.5727(2),b=0.9268(3),c=1.4666(4)nm,a=88.12(1)°,β=88.54(1)°,γ=80.82(1)°,V=0.7679(4)nm3,Z=1,DC=1.126Mg·m-3,F(000)=286,μ(MoKα)=0.69cm-1,R=0.048,wR=0.140.This compound had a centrosymmetrical structure.
文摘Benzoxazinone usually exists in many kinds of plants.It is applied in prepharmacy synthesis,and bioactivity studies,and has been prepared from O-aminophenol and chrol-with alkine and solvent by refluxing for a long time.In this work,2,2’-diphenyl-1,4-benzoxazin-3(4H)-one was solvent-free synthesized under microwave irradiation.The configuration and conformation of the product were determined by 1H NMR,IR,MS,elementary analysis and X-ray crystal analysis.The results of X-ray crystal analysis show that the compound crystallizes in a triclinic system,space group %P%1,cell parameter %a%=0.840 7(1)nm,%b%=0.845 1(1)nm,%c%=2.254 1(3)nm,%α%=96.111(3)°,%β%=97.196(3)°,%γ%=90.229(3)°,%V%= 1^579 6(4)nm3,%Z%=4,%D%c =1.267 Mg/m3,%F%(000)= 632.0,%μ%= 0.08 mm-1.In the compound,oxazinone ring is shown chair conformation,two benzene rings is placed in two sides of oxazinone ring distortedly.In crystal state,a centrosymmetric dimmer is formed %via% hydrogen bonds generated from amides of two near molecules.The benzene rings in a same chemical environment are paralleled by a distance of 0.260 9 nm.It displays aromatic π-π stacking interactions.