The crystal of the title compound (C_ 11H_ 11NOS_2, M_r =237.33) has been prepared and determined by X-ray single crystal diffraction. The crystal is monoclinic, space group P2_1/c with parameters : a=5.484 (1),...The crystal of the title compound (C_ 11H_ 11NOS_2, M_r =237.33) has been prepared and determined by X-ray single crystal diffraction. The crystal is monoclinic, space group P2_1/c with parameters : a=5.484 (1), b=7.793(2), c=28.295(6), β=90.277(4)°, V=1209.2(5)3, Z=4, D_c=1.034 g/cm3, μ(MoKα)= 0.413 mm -1, F(000)=496, the final R=0.0390 and wR=0.1051 for 1500 observed reflections with I>2σ(I). The X-ray analysis result shows that the orientation of methylsulfinyl and phenyl is the cis and confirms the E-stereochemistry of the title compound.展开更多
Microwave Assisted Organic Synthesis (MAOS) is energy efficient and effective tool to speed up the synthesis for drug discovery process. In the present study we report a novel protocol for the rapid, high throughput s...Microwave Assisted Organic Synthesis (MAOS) is energy efficient and effective tool to speed up the synthesis for drug discovery process. In the present study we report a novel protocol for the rapid, high throughput synthesis of mononuclear 2-amino-5-cyano-4,6-disubstituted pyrimidines, adaptable to parallel synthesis for compound libraries. The overall reaction time in hrs has been reduced to 25 - 50 minutes with improved yields.展开更多
建立了核磁共振氟谱法测定氰化物的氟化衍生化合物1-氰基-2,2,2-三氟-1-苯乙基乙酸酯(CTPA)含量的方法。以乙酸3-氟苄酯为内标,采用5mm Auto XBB探头,探头温度298.2K,考察了不同浓度化合物的定量条件;通过比较化合物样品定量峰与内标物...建立了核磁共振氟谱法测定氰化物的氟化衍生化合物1-氰基-2,2,2-三氟-1-苯乙基乙酸酯(CTPA)含量的方法。以乙酸3-氟苄酯为内标,采用5mm Auto XBB探头,探头温度298.2K,考察了不同浓度化合物的定量条件;通过比较化合物样品定量峰与内标物质响应峰面积,计算化合物的含量。结果该化合物的19 F-NMR检测方法在0.5~50μg/mL具有良好的线性(r2=0.9966),该方法的定量限0.5μg/mL,检出限0.2μg/mL;同时考察了该化合物在不同浓度下的测量准确度。展开更多
基金ProjectsupportedbytheNNSFofChina (No .2 9772 0 2 0 )
文摘The crystal of the title compound (C_ 11H_ 11NOS_2, M_r =237.33) has been prepared and determined by X-ray single crystal diffraction. The crystal is monoclinic, space group P2_1/c with parameters : a=5.484 (1), b=7.793(2), c=28.295(6), β=90.277(4)°, V=1209.2(5)3, Z=4, D_c=1.034 g/cm3, μ(MoKα)= 0.413 mm -1, F(000)=496, the final R=0.0390 and wR=0.1051 for 1500 observed reflections with I>2σ(I). The X-ray analysis result shows that the orientation of methylsulfinyl and phenyl is the cis and confirms the E-stereochemistry of the title compound.
文摘Microwave Assisted Organic Synthesis (MAOS) is energy efficient and effective tool to speed up the synthesis for drug discovery process. In the present study we report a novel protocol for the rapid, high throughput synthesis of mononuclear 2-amino-5-cyano-4,6-disubstituted pyrimidines, adaptable to parallel synthesis for compound libraries. The overall reaction time in hrs has been reduced to 25 - 50 minutes with improved yields.
文摘建立了核磁共振氟谱法测定氰化物的氟化衍生化合物1-氰基-2,2,2-三氟-1-苯乙基乙酸酯(CTPA)含量的方法。以乙酸3-氟苄酯为内标,采用5mm Auto XBB探头,探头温度298.2K,考察了不同浓度化合物的定量条件;通过比较化合物样品定量峰与内标物质响应峰面积,计算化合物的含量。结果该化合物的19 F-NMR检测方法在0.5~50μg/mL具有良好的线性(r2=0.9966),该方法的定量限0.5μg/mL,检出限0.2μg/mL;同时考察了该化合物在不同浓度下的测量准确度。
