3-Deoxy-3-(p-fluorine-phenylamino)-1,2-O-isopropylidene-α-D-ribofuranose 3 was synthesized and characterized by IR, NMR and HRMS, and its crystal structure was determined by X-ray diffraction analysis. Crystal data for 3: monoclinic, space group P21, a = 7.0403(14), b = 6.7780(4), c = 14.932(3) A, β = 94.74(3)°, C14H18FNO4, Mr = 283.29, V = 710.1(2) ·3, Z = 2, Dc = 1.325 g/cm3, μ = 0.105 mm-1, F(000) = 300, the final R = 0.0468 and wR = 0.0926 for 1969 observed reflections (I > 2σ(I)). Two intermolecular hydrogen bonds are observed. The absolute configuration of this molecule was confirmed by comparison with that of the original material.
The title compound 3 was synthesized and characterized by IR,NMR and H-RMS,and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic system (C16H23NO7S,Mr=373.41),space group P21,with a=12.000(2),b=5.5970(11),c=13.689(3),β=93.25(3)°,V=917.9(3)3,Z=2,Dc=1.351 g/cm3,F(000)=396,μ=0.213 mm-1,the final R=0.0489 and wR=0.0777 for observed reflections (I > 2σ(I)). Three intramolecular and three intermolecular hydrogen bonds were found. The absolute configuration of this molecule was confirmed by comparing with the original material.
1,2-O-Isopropylidene-5-O-p-toluenesulfonyl-α-D-erythro-pentofuranos-3-ulose 1 was treated with thiourea and aminothiourea to give a D-ribose derivative 2 bearing a 2-amino 1,3-thiazine ring and a thiosemicarbazone derivative 5, respectively. 2 was acylated with Ac2O and propandioic acid to afford two acylation derivatives 3 and 4, respectively. Reduction of 5 with NaBH4 in methanol produced a hydrothiosemicarbazone derivative 6. The absolute configuration of 2 was confirmed by X-ray crystallographic analysis. The structures of all products were elucidated by IR, NMR and HRMS spectra.
<正>It was reported that steroidal lactones possess useful biological activities such as anticancer, antibacter...
LI, He-Ping SHAN, Li-Hong HUANG, Li-Hua LIU, Hong-Min (New Drug Research and Development Center, Department of Chemistry, Zhengzhou University, Zhengzhou 450052)
<正>Andrographolide (1) is one of the major labdane diterpenoidal constituents of Andrographis panicutate (Burm...
XU,Hai-Wei LIU, Su WANG, Tun-Feng LIU, Hong-Min (New Drug Research & Development Center, Department of Chemistry, Zhengzhou University, Zhengzhou 450052)