The novel spirophosphoroheterocycle (C14H19N2OPS2, Mr = 326.40) was synthesized by the treatment of Lawesson磗 reagent with amino cyclohexanenitrile, and its crystal structure was analyzed by X-ray diffraction method....The novel spirophosphoroheterocycle (C14H19N2OPS2, Mr = 326.40) was synthesized by the treatment of Lawesson磗 reagent with amino cyclohexanenitrile, and its crystal structure was analyzed by X-ray diffraction method. The title compound is of monoclinic, space group P21/n with a = 14.296(4), b = 11.028(3), c = 21.715(6) ? ?= 101.823(6), V = 3351.1(2) 3, Z = 8, Dc = 1.294 g/cm3, ?= 0.71073 ? (MoK? = 0.410 mm―1 and F(000) = 1376. The structure was refined to R = 0.0521 and wR = 0.0744 for 5909 observed reflections with I > 2(I). X-ray diffraction analysis reveals that there are three rings in the molecule. The saturated 6-membered ring presents in chair conformation and the 5-membered phosphoroheterocycle is planar. The molecules are found to exist in couples. The existence of d-p?bonds between P and two N atoms and the intermolecular hydrogen bonds are found as well.展开更多
A novel asymmetric[4+2]cycloaddition of 2-methylidenetrimethylene carbonate with pyrrolidonederived enones has been achieved to produce the functionalized tetrahydropyran-fused spirocyclic scaffolds via palladium-cata...A novel asymmetric[4+2]cycloaddition of 2-methylidenetrimethylene carbonate with pyrrolidonederived enones has been achieved to produce the functionalized tetrahydropyran-fused spirocyclic scaffolds via palladium-catalysis.An array of enantioenriched spiro-pyrrolidine-2,3-diones bearing adjacent quaternary and tertiary stereocenters are obtained in high yields with excellent enantioselectivities(up to 96% yield and 99% ee).The further transformation of the product has been accomplished for the construction of medical interesting β^(2,2)-amino acids and β-lactams.Preliminary mechanistic research was well conducted.展开更多
The 1,3-dipolar cycloaddition of an azomethine ylide generated by a decarboxylative route from sarcosine and acenaphthenequinone to 7-arylmethylidene-3-aryl-3,4-dihydro-2H-thiazolo[3,2-aJ[1,3,5]triazin-6（7H）-ones af...The 1,3-dipolar cycloaddition of an azomethine ylide generated by a decarboxylative route from sarcosine and acenaphthenequinone to 7-arylmethylidene-3-aryl-3,4-dihydro-2H-thiazolo[3,2-aJ[1,3,5]triazin-6（7H）-ones afforded novel dispiro[acenaphthylene-1,2’-pyrrolidine]-3＇,7″-[1,3]thiazolo[3,2-a][1,3,5]triazines in moderate yields. The structures of the products were determined and characterized thoroughly by NMR, MS, IR, elemental analysis and X-ray crystallographic analysis. The results of experiment indicated that this 1,3-dipolar cycloaddition proceeded with high stereoselectivity and regioselectivity.展开更多
文摘The novel spirophosphoroheterocycle (C14H19N2OPS2, Mr = 326.40) was synthesized by the treatment of Lawesson磗 reagent with amino cyclohexanenitrile, and its crystal structure was analyzed by X-ray diffraction method. The title compound is of monoclinic, space group P21/n with a = 14.296(4), b = 11.028(3), c = 21.715(6) ? ?= 101.823(6), V = 3351.1(2) 3, Z = 8, Dc = 1.294 g/cm3, ?= 0.71073 ? (MoK? = 0.410 mm―1 and F(000) = 1376. The structure was refined to R = 0.0521 and wR = 0.0744 for 5909 observed reflections with I > 2(I). X-ray diffraction analysis reveals that there are three rings in the molecule. The saturated 6-membered ring presents in chair conformation and the 5-membered phosphoroheterocycle is planar. The molecules are found to exist in couples. The existence of d-p?bonds between P and two N atoms and the intermolecular hydrogen bonds are found as well.
基金Financial support from the National Key Research and Development Program of China(No.2021YFF0600704)。
文摘A novel asymmetric[4+2]cycloaddition of 2-methylidenetrimethylene carbonate with pyrrolidonederived enones has been achieved to produce the functionalized tetrahydropyran-fused spirocyclic scaffolds via palladium-catalysis.An array of enantioenriched spiro-pyrrolidine-2,3-diones bearing adjacent quaternary and tertiary stereocenters are obtained in high yields with excellent enantioselectivities(up to 96% yield and 99% ee).The further transformation of the product has been accomplished for the construction of medical interesting β^(2,2)-amino acids and β-lactams.Preliminary mechanistic research was well conducted.
基金Project supported by the National Natural Science Foundation of China （Nos. 20971041, 20803020, 20772027）, the Key Project of Chinese Ministry of Education （No. 210146） and Scientific Research Fund of Hunan Provincial Education Department （Nos. 09B032, 09C385, 09K081）.
文摘The 1,3-dipolar cycloaddition of an azomethine ylide generated by a decarboxylative route from sarcosine and acenaphthenequinone to 7-arylmethylidene-3-aryl-3,4-dihydro-2H-thiazolo[3,2-aJ[1,3,5]triazin-6（7H）-ones afforded novel dispiro[acenaphthylene-1,2’-pyrrolidine]-3＇,7″-[1,3]thiazolo[3,2-a][1,3,5]triazines in moderate yields. The structures of the products were determined and characterized thoroughly by NMR, MS, IR, elemental analysis and X-ray crystallographic analysis. The results of experiment indicated that this 1,3-dipolar cycloaddition proceeded with high stereoselectivity and regioselectivity.
