Ph 2NH and PCl 3 interacted at a molar ratio of 1∶1 05 and slow elevated temperature and then at 210-220 ℃ for 6 h. The brown solution obtained was treated with H 2O to produce a very hard brown solid believed to be...Ph 2NH and PCl 3 interacted at a molar ratio of 1∶1 05 and slow elevated temperature and then at 210-220 ℃ for 6 h. The brown solution obtained was treated with H 2O to produce a very hard brown solid believed to be a mixture of 5,10 dihydrophenophosphazine 10 oxide(1a) and 10,10(5H,5H) spirobipenophosphazinium chloride(1b). This brown solid was directly oxidized with peracetic acid in HOAc prior to the separation of them to give compound 10 hydroxy 5,10 dihydropheno phosphazine 10 oxide(2) with a higher yield(45%) than that of the literature(27%). When treated with excess SOCl 2, compound 2 could quantitatively be converted to the corresponding phosphinyl chloride and the latter could further be transformed into 10 methoxy 5,10 dihydrophenophosphazine 10 oxide in 70% as treated with NaOMe in methanol. Compound 2 could also be converted to a bisanion when treated with NaH in DMF. The resulted bisanion reacted with MeI to give 5 methyl 10 hydroxy 5,10 dihydrophenophosphazine 10 oxide in a 73% yield which would be converted to 5 methyl 10 methoxy 5,10 dihydrophenophosphazine 10 oxide in a 56% yield by the same way of synthesizing 10 methoxy 5,10 dihydrophenophosphazine 10 oxide. All these compounds obtained were identified by surveying their melting points, and spectra and elemental analysis.展开更多
基金Supported by National Natural Science Foundation of China(No.2 9972 0 0 6 ) .
文摘Ph 2NH and PCl 3 interacted at a molar ratio of 1∶1 05 and slow elevated temperature and then at 210-220 ℃ for 6 h. The brown solution obtained was treated with H 2O to produce a very hard brown solid believed to be a mixture of 5,10 dihydrophenophosphazine 10 oxide(1a) and 10,10(5H,5H) spirobipenophosphazinium chloride(1b). This brown solid was directly oxidized with peracetic acid in HOAc prior to the separation of them to give compound 10 hydroxy 5,10 dihydropheno phosphazine 10 oxide(2) with a higher yield(45%) than that of the literature(27%). When treated with excess SOCl 2, compound 2 could quantitatively be converted to the corresponding phosphinyl chloride and the latter could further be transformed into 10 methoxy 5,10 dihydrophenophosphazine 10 oxide in 70% as treated with NaOMe in methanol. Compound 2 could also be converted to a bisanion when treated with NaH in DMF. The resulted bisanion reacted with MeI to give 5 methyl 10 hydroxy 5,10 dihydrophenophosphazine 10 oxide in a 73% yield which would be converted to 5 methyl 10 methoxy 5,10 dihydrophenophosphazine 10 oxide in a 56% yield by the same way of synthesizing 10 methoxy 5,10 dihydrophenophosphazine 10 oxide. All these compounds obtained were identified by surveying their melting points, and spectra and elemental analysis.
文摘目的探究血清瓜氨酸组蛋白H3(citrullinated histone H3,CitH3)、降钙素原(procalcitonin,PCT)及白细胞介素-10(interleukin-10,IL-10)对体外心肺复苏(extracorporeal cardiopulmonary resuscitation,ECPR)后急性肺损伤(acute lung injury,ALI)的预测价值。方法择取2021年1月至2024年4月行ECPR的患者126例,入院次日空腹采血测定患者血清CitH3、PCT、IL⁃10水平。根据ECPR后ALI发生与否分为ALI组与非ALI组,对比两组临床资料及血清CitH3、PCT、IL-10水平,Logistic多因素回归分析ECPR后ALI发生的危险因素。另外受试者工作特征(receive operating characteristic,ROC)曲线分析血清CitH3、PCT、IL-10对ALI的预测价值。结果因6例患者未配合完成相关检查等被剔除,最终纳入120例患者,其中住院期间ALI发生28例(ALI组),ALI未发生92例(非ALI组)。ALI组入院时急性生理学和慢性健康状况评分(Acute Physiology and Chronic Health Scoring System,APACHEⅡ)、序贯器官衰竭评估(Sequential Organ Failure Assessment,SOFA)、心肺复苏到自主循环恢复时间均大于非ALI组(P<0.05);ALI组血清CitH3、PCT、IL-10水平均高于非ALI组(P<0.05)。Logistic多因素回归分析显示心肺复苏到自主循环恢复时间、血清CitH3、PCT及IL-10是ALI发生的独立危险因素(P<0.05)。ROC曲线显示,血清CitH3、PCT、IL-10单一及3项联合预测ALI发生的曲线下面积(area under curve,AUC)分别为0.886、0.837、0.852、0.951,3项联合的AUC均大于PCT、IL-10单一检测(P<0.05)。结论ECPR后ALI发生患者血清CitH3、PCT、IL-10水平上升,对ALI发生有一定的预测价值,特别是联合检测效能更显著。