The title compound N-（7-chloro-5-ethoxy-2H-[1,2,4]thiadiazolo[2,3-a]pyrimidin- 2-ylidene）- 2-（2,4-dichlorophenoxy）propanamide 3 has been synthesized through using bromine as cyclic reagent in 63% isolated yield. Suitable single crystals for X-ray diffraction were obtained by recrystallization from the mixture solvents at room temperature. Crystallographic data of 3： C 16H13C13O3S, Mr = 447.71, triclinic, space group P1, a = 8.7461（8）, b = 9.9560（10）, c = 11.8572（11） A, a = 94.341（2）, β = 94.683（2）, γ = 112.929（2）°, Z = 2, V= 941.21（15） A^3, Dc = 1.580 g/cm^3, F（000） = 456, R = 0.0794, wR = 0.2056 andμ（MoKa） = 0.623 mm^-1. The title compound 3 was found to be effective in herbicidal activity.
Two novel chiral BINOL derivatives with bis（benzylamine） groups at the 3,3- positions have been synthesized through the condensation reaction between 2,2＇-bis（methoxymethyleneoxy）-1,1＇-binaphthyl-3,3＇-dicarboxylic acid and benzylamine or N-phenyl benzylamine in the presence of triethylamine. Suitable single crystal of （R）-N,N＇-dibenzyl-2,2＇-dihydroxy-1, 1＇-binaphthly-3,3＇-diformamide （R）-3 for X-ray diffraction was obtained by recrystallization at room temperature from the mixture solvents. Crystallographic data of （R）-3： C40H36N2O6, Mr = 640.71, monoclinic, space group P21, a = 6.746（3）, b = 21.883（9）, c = 11.723（5）A,β = 104.605（7）°, Z= 2, V= 1674.7（12）A^3, Dc = 1.271 g/cm^3, F（000） = 676, R = 0.0729, wR = 0.1687 andμ（MoKa） = 0.086 mm^-1. Two chiral BINOL ligands were found to be effective in the enantioselective addition of diethylzinc to aldehydes and much different enantioselectivity was observed both in the presence and absence of Ti（Oipr）4. in the former case, （R）-3 showed moderate enantioselectivity, which was lower than that of （R）-BINOL＇s; and in the latter case, （R）-4 gave the highest enantioselectivity up to 93.3% ee.
The title compound N-（5,7-dimethoxy-2H-[1,2,4]thiadiazolo[2,3-a]pyrimidin-2- ylidene）-2-（2,4-dichlorophenoxy）propanamide 3 has been synthesized through using bromine as cyclic reagent in 66% isolated yield. Suitable single crystals for X-ray diffraction were obtained by recrystallization from the mixture solvents at room temperature. Crystallographic data of 3： C32H28Ci4N8O9S2, Mr = 874.56, monoclinic, space group P21/c, a = 18.612（8）, b = 14.084（6）, c = 14.757（6） A, α = 90.00, β = 95.505（7）, ）, = 90.00°, Z = 4, V= 3850（3） A^3, Dc = 1.509 g/cm^3, F（000） = 1792, R = 0.0704, wR = 0.1454 and ° = 0.479 mm^-1. The title compound 3 was found to be effective in herbicidal activity.
The title compound （R）-3,3＇-bis（benzyloxymethyl）-1,1＇-bi-2,2＇-naphthol （R）-3 has been synthesized through the deprotection of MOM group by iprOH/HCl in 83% isolated yield and the suitable single crystals for X-ray diffraction were obtained by recrystallization at room temperature from the mixture solvents. Crystallographic data for （R）-3： C36H30O4, Mr = 526.60, triclinic, space group P1, a = 10.057（6）, b = 11.934（7）, c = 12.314（6） A, α = 85.52（2）, β = 70.245（13）, γ = 76.554（11）°, Z= 2, V 1352.8（13） A^3, Dc = 1.293 g/cm^3, F（000） = 556, R = 0.0745, wR = 0.1933 and #（MoKa） = 0.083 mm^-1. The title compound （R）-3 was found to be effective in the enantioselective addition of diethylzinc to aldehydes both in the presence and absence of Ti（Oipr）4. In the latter case, （R）-3 showed much higher catalytic activity and enantioselectivity than （R）-BINOL＇s.
LIU Guo-Hua YU Han XUE Yun-Ning YAO Mei FANG Hai-Bin
Nano-carbon materials were synthesized by the catalytic decomposition of acetylene at 400℃ by using Fe/Al2O3 as catalyst. The product was refluxed in 36% concentrated HCl at 60℃ for 48 h in order to re-move the catalyst support. The samples were examined by scanning and high resolution transmission electron microscopy,energy dispersive spectroscopy and X-ray diffraction. The results show that nano onion-like fullerenes encapsulating a Fe3C core were obtained. These had a structure of stacked graphitic fragments,with diameters ranging from 15―50 nm. When the product was further heat-treated at 1100℃ for 2 h,nano onion-like fullerenes with a clear concentric graphitic layer structure were obtained. The growth mechanism of nano onion-like fullerenes encapsulating metal cores is suggested to follow a vapor-solid growth model.
LIU XuGuang1,2,WANG CunJing1,2,YANG YongZhen1,3,GUO XingMei1,2,WEN HaiRong1,2 & XU BingShe1,3 1 Key Laboratory of Interface Science and Engineering in Advanced Materials,Ministry of Education,Taiyuan University of Tech-nology,Taiyuan 030024,China
