N－甲基吡咯烷酮、α－吡咯烷酮合成物系气相色谱分析

Ｎ－甲基吡咯烷酮、α－吡咯烷酮合成物系气相色谱分析邱立勤，米镇涛，张香文（天津大学天津石油化工技术开发中心天津３０００７２）１前言Ｎ－甲基吡咯烷酮（ＮＭＰ）具有高极性、高化学稳定性及热稳定性，是重要的工业溶剂，可广泛应用于有机化合物萃取、润滑油精制、...     

N－甲基吡咯烷酮、α－吡咯烷酮合成物系气相色谱分析

 This paper describes a GC analytical method in the synthes is of N-methyl pyrrolidone of a-pyrrolidone.This procedure was performed with a column packed with 6%OV-17/silanized 101 support and FID detec-tor. Calibration factors and detection conditions are given,The coefficients of variation of NMP and a-P were0.6%and 0.5%respectively. The relative errors of all the components were not more than±3.0%,Thequantitative analysis is fast,simple and accurate.     

毛细管气相色谱,色谱—质谱联用测定金刚烷及其异构体

本文给出了金刚烷及其异构体合物系毛细管气相色谱及色谱－质谱联用分析方法，色谱柱为ＣＢＰＩ键合石英毛细管、氢火焰检则器。列出了标准曲线和检测条件，回收率为９８．３％－１０１．２％，相对标准偏差〈４．０％，本方法定量分析快速、简便、准确。     

有机天然产物化学实验的教学改革与实践

Natural product chemistry experiments, which train the students to master the basic skills for extraction, separation and identification of the active components of natural products, and acquaint with the research methods of natural product chemistry, are an important part of organic chemistry laboratory. This paper analyzes the common problems related to the current natural products chemistry laboratories in domestic universities. In recent years, we carried out the reforms of the teaching contents, teaching conditions, and teaching methods. The teaching practices show that the students' learning interest and efficiency, the abilities to analyze and solve problems, and the scientific research abilities have been trained and strengthened. The teachers' experimental teaching level and teaching quality have been greatly improved.     

戊二醛合成体系气相色谱分析

本文给出了环戊烯合成戊二醛体系的气相色谱分析方法，色谱柱为硅烷化担体载１０％ＰＥＧ－２０Ｍ固定液，氢火焰检测器，列出了标准曲线和检测条件，变异系数均〈１．５％，相对误差±２．０％以内，该定量分析快速，简便，准确。     

铱催化的MBH乙酸酯与吲哚酮类化合物的烯丙基化反应

研究了一种新的铱催化的Morita-Baylis-Hillman(MBH)乙酸酯与3-苯基取代的吲哚酮的烯丙基烷基化反应, 发现铱催化的区域选择明显不同于钯催化的反应, 直接、 高效地合成了一类未见报道的具有新结构的 3,3-二取代的吲哚酮类化合物. 通过对亚磷酰胺、 双膦及单膦等配体、 金属源、 溶剂、 碱以及反应温度的筛选, 获得了适合该反应的催化体系及最优条件: 以[Ir(COD)Cl]₂(摩尔分数5%)和亚磷酰胺配体(L6, 摩尔分数10%)为催化剂, CH₃CN为溶剂, Cs₂CO₃为碱, 于?30 ℃反应25 h. 在最优条件下, 对不同类型取代基的底物进行了考察, 发现底物普适性良好, 产率最低为84%, 最高可达98%. 同时还发现, 底物取代基的电性对反应产率影响不大, 一些其它类型的双膦和单膦配体对催化反应也有较好的催化效果.