The title compound 4-（4,6-dimethoxylpyrimidin-2-yl）-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in eth...The title compound 4-（4,6-dimethoxylpyrimidin-2-yl）-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at the room temperature. The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis＇ Crystallographic data： C9H12N4O4S, Mr = 272.29, monoclinic, space group C2/m with a = 1.6672（3）, b = 0.66383（12）, c = 1.1617（2） nm, β = 109.275（2）°, V = 1.2136（4） nm^3, Dc = 1.490 g/cm^3,μ = 0.281 mm^-1, F（000） = 568, Z = 4, R1 = 0.0341and wR2 = 0.1042.展开更多
The synthesis of 99-acetoxy-3(4), 11(13)-dien-5αH 7αH-12-eudesmanoic acid methyl ester (2) was achieved from oxycarvone. The key step is the p-toluenesulfonhydrazide assisted reductiv rearrangement reaction
以4-氨基-3-甲基苯甲酸为起始原料,经混酸硝化反应、正丁酸酐酰化反应和甲醇酯化反应等三步合成目标产物3-甲基-4-正丁酰氨基-5-硝基苯甲酸甲酯.其中间产物和目标产物的化学结构均经1 H NMR、13 C NMR、MS等方法进行了表征.实验过程中...以4-氨基-3-甲基苯甲酸为起始原料,经混酸硝化反应、正丁酸酐酰化反应和甲醇酯化反应等三步合成目标产物3-甲基-4-正丁酰氨基-5-硝基苯甲酸甲酯.其中间产物和目标产物的化学结构均经1 H NMR、13 C NMR、MS等方法进行了表征.实验过程中还对各步反应条件进行了优化,各步在最佳反应条件下总产率可达72.6%.该合成路线简单易行,容易实现工业化生产,具有很好的应用价值.展开更多
基金This work was supported by the National Natural Science Foundation of China (20571060) and Education Committee of Shaan Xi Province (05JK294)
文摘The title compound 4-（4,6-dimethoxylpyrimidin-2-yl）-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at the room temperature. The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis＇ Crystallographic data： C9H12N4O4S, Mr = 272.29, monoclinic, space group C2/m with a = 1.6672（3）, b = 0.66383（12）, c = 1.1617（2） nm, β = 109.275（2）°, V = 1.2136（4） nm^3, Dc = 1.490 g/cm^3,μ = 0.281 mm^-1, F（000） = 568, Z = 4, R1 = 0.0341and wR2 = 0.1042.
文摘The synthesis of 99-acetoxy-3(4), 11(13)-dien-5αH 7αH-12-eudesmanoic acid methyl ester (2) was achieved from oxycarvone. The key step is the p-toluenesulfonhydrazide assisted reductiv rearrangement reaction
文摘以4-氨基-3-甲基苯甲酸为起始原料,经混酸硝化反应、正丁酸酐酰化反应和甲醇酯化反应等三步合成目标产物3-甲基-4-正丁酰氨基-5-硝基苯甲酸甲酯.其中间产物和目标产物的化学结构均经1 H NMR、13 C NMR、MS等方法进行了表征.实验过程中还对各步反应条件进行了优化,各步在最佳反应条件下总产率可达72.6%.该合成路线简单易行,容易实现工业化生产,具有很好的应用价值.
