The synthesis of a novel host blocked in the cone conformation and bearing m-methoxycarbonylbenzyl groups at the lower rim is described. X-ray crystal structure analysis revealed that action of one molecule of compoun...The synthesis of a novel host blocked in the cone conformation and bearing m-methoxycarbonylbenzyl groups at the lower rim is described. X-ray crystal structure analysis revealed that action of one molecule of compound upon one molecule of CH 3CN or one molecule of CH 3NO 2, forms an intramolecular inclusion complex, respectively, by CH 3-π interactions. The complex of L with tetrabutyl ammonium bromide(TBAB), L·TBAB, was obtained. The results of DTA-TG and XRD analysis of L·TBAB can also be considered as an intramolecular inclusion complex.展开更多
以4-氟-3-甲基苯胺为原料,经重氮化、甲基化和溴化、水解等四步反应合成2-氟-5-甲氧基苯甲醛,产物的含量为99.176%(HPLC),总摩尔产率约37%,产物结构通过了1 H NMR和MS的验证。其中,重氮化酸性水解反应的最佳条件为n(4-氟-3-甲基苯胺)∶n...以4-氟-3-甲基苯胺为原料,经重氮化、甲基化和溴化、水解等四步反应合成2-氟-5-甲氧基苯甲醛,产物的含量为99.176%(HPLC),总摩尔产率约37%,产物结构通过了1 H NMR和MS的验证。其中,重氮化酸性水解反应的最佳条件为n(4-氟-3-甲基苯胺)∶n(水)∶n(磷酸)∶n(五水硫酸铜)=1∶30∶4.0∶1.1,甲基化反应的最佳反应条件为n(4-氟-3-甲基苯酚)∶n(硫酸二甲酯)=1∶1.3,NaOH水溶液的质量浓度为20%,反应时间约为10h。该法具有生产成本低、反应条件温和、易于工业化生产等优点。展开更多
文摘The synthesis of a novel host blocked in the cone conformation and bearing m-methoxycarbonylbenzyl groups at the lower rim is described. X-ray crystal structure analysis revealed that action of one molecule of compound upon one molecule of CH 3CN or one molecule of CH 3NO 2, forms an intramolecular inclusion complex, respectively, by CH 3-π interactions. The complex of L with tetrabutyl ammonium bromide(TBAB), L·TBAB, was obtained. The results of DTA-TG and XRD analysis of L·TBAB can also be considered as an intramolecular inclusion complex.
文摘以4-氟-3-甲基苯胺为原料,经重氮化、甲基化和溴化、水解等四步反应合成2-氟-5-甲氧基苯甲醛,产物的含量为99.176%(HPLC),总摩尔产率约37%,产物结构通过了1 H NMR和MS的验证。其中,重氮化酸性水解反应的最佳条件为n(4-氟-3-甲基苯胺)∶n(水)∶n(磷酸)∶n(五水硫酸铜)=1∶30∶4.0∶1.1,甲基化反应的最佳反应条件为n(4-氟-3-甲基苯酚)∶n(硫酸二甲酯)=1∶1.3,NaOH水溶液的质量浓度为20%,反应时间约为10h。该法具有生产成本低、反应条件温和、易于工业化生产等优点。
