A series of new thiazoline derivatives 2-alkyl（aryl） imino-4-amino-5-ethoxycarbonyl-3-phenyl-3H- thiazoline （3） and bis（2-imino-4-amino-5-ethoxycarbonyl-3-phenyl-3H-thiazoline alkylene （4） have been synthesized by reactions of intermediate 4-amino-5-ethoxycarbonyl-2-methylthio-3-phenyl-3H- thiazolinium sulphate （2） with alkylamines or arylamine in 64%-89% yields. The structures of 3 and 4 have been confirmed by 1H NMR, El-MS, IR spectroscopy and elemental analyses. Some compounds exhibited high or moderate herbicidal activities against the roots of rapeseed and barnyard grass at 100 mg/L.
选择2,4-二氯苯氧乙酸为起始原料,经氯化亚砜氯化后得2,4-二氯苯氧乙酰氯2,与不同取代的α-羟基烃基膦酸酯反应制备关键中间体3,再与碘化钠反应,合成了6个未见文献报道的O-烷基α-(2,4-二氯苯氧乙酰氧基)烃基膦酸钠4.通过1 H NMR,IR和元素分析对所合成的化合物进行了结构表征,其中4f经过MS进一步确证.初步的生物活性测试结果表明:目标化合物具有较高的除草活性,在10μg/g的浓度下,化合物4a^4e对稗草和油菜根的抑制率均达到了90%以上.
A new crystal of 4-fluoro-N-（2-methyl-5-（（2-（p-tolyloxy）acetamido）methyl）pyrimi- din-4-yl）benzamide has been prepared at room temperature and characterized by 1H NMR, 13C- NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic, space group P21 /c with a = 17.226（5）, b = 13.934（4）, c = 17.262（5）, μ= 92.180（5）°, V = 4140（2） ？3, Dc = 1.311 g/cm3, Z = 8, F（000） = 1712 and ？？= 0.095 mm-1. The molecular packing in the crystal is the result of N-H…ydrogen bonds.
A new crystal of（E）-2-（2,4-dichlorophenoxy）-1-（5,5-dimethyl-2-oxido-1,3,2-dioxaphosphinan-2-yl）vinyl 2-（2,4-dichlorophenoxy）acetate has been determined by single-crystal X-ray diffraction. The compound crystallizes in triclinic, space group P1 with a = 7.9393（17）, b = 11.974（3） ？, c = 13.532（3） ？, α = 90.937（4）, β = 101.998（3）, γ = 101.363（4）°, V = 1231.5（5） ？3, Dc = 1.500 Mg/m3, Z = 2, F（000） = 568 and μ = 0.585 mm^（-1）. The molecular packing in the crystal is the result of C（10）–H（10）···O（5） hydrogen bond, as well as weak π-π stacking interactions. The herbicidal activity results indicated that the title compound 3 showed 80~100% inhibitory activities against all of the tested weeds at a dosage of 150 g×ai/ha.
A new crystal of 2-methylpropan-2-aminium methyl （（4-fluorobenzamido）（4- fluorophenyl）methyl）phosphonate has been prepared at room temperature and characterized by ZH- NMR, 13C NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic space, group C2/c with a = 20.719（2）, b = 11.8559（13）, c = 18.176（2） A,β = 94.434（2）°, V= 4451.4（9） A3, Dc = 1.317 Mg/m3, Z= 8, F（000） = 1864 and μ= 0.174 mm-1. The crystal packing is stabilized by intermolecular N-H……O and O-H……O hydrogen bonds, as well as by weak π-π stacking interactions.
选择硫脲为起始原料,与溴乙酸乙酯一步反应生成2-亚氨基-4-噻唑烷酮(2),与苯甲醛缩合得2-氨基-5-苯甲叉基-4-噻唑酮(3),再与取代苯甲酰氯反应,合成了7个未见文献报道的噻唑酮类化合物.通过IR,1 H NMR,13 C NMR和元素分析对目标化合物进行了结构鉴定,测定了它们的抗肿瘤活性和杀菌活性.结果表明:部分测试化合物对肿瘤细胞KB和CNE2有一定的抑制作用,化合物4a对6种病菌都有不同程度的抑制活性.
