甲磺酸铜催化合成草酸二异戊酯

制备了甲磺酸铜催化剂,对其结构进行了IR和热重分析,并用于催化草酸和异戊醇的酯化反应。结果表明,甲磺酸铜具有催化活性高、稳定,易分离,重复使用性能优良,对环境友好的特点。最佳酯化工艺条件为:n(异戊醇):n(草酸)=2．8:1,w(甲磺酸铜)=0．3％,以过量的异戊醇为带水剂,回流反应2．0 h,酯化率可达到96．8％。     

甲基磺酸镧催化缩醛化反应性能的研究

以正辛醛和乙二醇为原料,甲基磺酸镧为催化剂,合成了正辛醛缩乙二醇。采用正交实验法考察了影响收率的因素。其最优条件为,正辛醛∶乙二醇∶催化剂∶带水剂为1m o l∶1.2m o l∶7.5g∶75mL,反应在回流温度下进行,反应时间3.0h,收率可达87.2%。用此方法合成了其它三种缩醛,同样获得满意结果。证明甲基磺酸镧对缩醛化反应具有较高的催化活性。     

Cation Effect on the Binary and Ternary Phase Behaviors of Double-Tailed Methanesulfonate Amphiphiles

A series of symmetrical dialkyl methanesulfonate amphiphiles [DiC _n CHSO ₃ ] _m M (n = 6, 7, 8) with different counter cations (M^m+ = H⁺, Li⁺, Na⁺, K⁺, Cu²⁺, Zn²⁺, Mg²⁺, Ca²⁺, Sc³⁺) were synthesized in five steps. Their solubility and critical micelle concentration (CMC) in water were determined highlighting a huge effect of the chain length and the nature of the cation. The hydrophilic–lipophilic balance of the surfactants were assessed with the phase inversion temperature (PIT)-slope method based on the deviation from the PIT of the reference C₁₀E₄/n-octane/0.01 M NaCl_(aq) emulsion through addition of increasing amounts of the dialkyl methanesulfonates. The hydrophilicity of the surfactants was thus ranked in terms of dPIT/dx_sulfonate. A “cation” scan with the [DiC ₆ CHSO ₃ ] _m M /benzene/water systems at f_w = 0.5 was finally performed confirming the hydrophilicity ranking obtained with the PIT-slope method. It revealed that the [DiC ₆ CHSO ₃ ] ₂ Mg behaves as a “Balanced Surfactant” able to form spontaneously a three-phase microemulsion system (Winsor III) just in the presence of water and oil, in the same way as the catalytic surfactant dimethyldioctylammonium molybdate, which has the same PIT-slope.     

高纯度甲基磺酸亚锡生产新工艺

研究了用锡和甲基磺酸反应直接生产电镀用的纯甲基磺酸亚锡的新工艺，其产品纯度达到99．5％以上，并研究了提高设备利用率和生产效率的措施，设备利用率可提高2．28倍，建成的150t/a甲基磺酸亚锡生产装置，其产品产量、质量均达到了预期效果。该工艺无毒无害无三废排放。     

隔膜电解法合成电镀级甲基磺酸亚锡

研究了隔膜电解法合成甲基磺酸亚锡的工艺。考察了电流密度、阴极酸质量浓度、阳极酸质量浓度、稳定剂的加入量、浓缩温度等因素对产品的影响。在电流密度1.8 A/dm2、常温反应60 h,阴极酸质量浓度180 g/L、阳极酸质量浓度180 g/L、浓缩温度80℃以下的条件下,锡的直收率92%以上,电流效率95%以上。     

食用香料柠檬醛缩1,2-丙二醇的新法合成

以柠檬醛和1,2-丙二醇为原料,甲基磺酸铜为催化剂,合成了柠檬醛缩1,2-丙二醇。考察了影响收率的因素。其最优条件为:柠檬醛∶1,2-丙二醇:催化剂∶带水剂为1mol:1.4mol∶24mmol∶100mL,反应在回流温度下进行,反应时间2.0h。收率可达88.6%。     

Anodic behavior of gold in 1-butyl-3-methylimidazolium methanesulfonate ionic liquid with chloride anion

The anodic behavior of gold has been investigated in presence of chloride and/or water in 1-butyl-3-methylimidazolium methanesulfonate (BMI CH₃SO₃) ionic liquid (IL). The cyclic voltammetry (CVs) in presence of chloride ions shows two waves attributed to the oxidation of the gold electrode which occurs under two steps: the first one is attributed to the electrochemical dissolution of gold into to gold(I), while the second one is attributed to an overlap of the chloride oxidation step as well as the oxidation of Au(I) to Au(III). Furthermore the determination of water and chloride content in IL allowed observing that the passive layer induced by water could be removed under chloride. Thanks to those results we were able to clarify the conditions of gold recovering in this kind of electrolyte.     

甲烷磺酸铝催化合成氯乙酸酯的性能研究

合成了甲烷磺酸铝,用热重和红外对其进行表征。并以甲烷磺酸铝为催化剂,研究其催化氯乙酸与异丙醇酯化反应中各种因素对酯化率的影响。反应条件为:醇酸摩尔比1.2∶1,催化剂摩尔分数1.0%(以酸的摩尔数计),反应时间2.5h,反应温度80～85℃,环己烷5mL作为带水剂,酯化率可达96.8%,反应后催化剂经过简单的相分离就可重复使用。与AlCl3·6H2O、Al2(SO4)3·18H2O及其它Lewis酸进行比较,甲烷磺酸铝的催化活性最好。用甲烷磺酸铝作催化剂合成其它氯乙酸酯,酯化率均在96.0%以上。     

The Alkylating Agent Methyl Methanesulfonate Triggers Lipid Alterations at the Inner Nuclear Membrane That Are Independent from Its DNA-Damaging Ability

In order to tackle the study of DNA repair pathways, the physical and chemical agents creating DNA damage, the genotoxins, are frequently employed. Despite their utility, their effects are rarely restricted to DNA, and therefore simultaneously harm other cell biomolecules. Methyl methanesulfonate (MMS) is an alkylating agent that acts on DNA by preferentially methylating guanine and adenine bases. It is broadly used both in basic genome stability research and as a model for mechanistic studies to understand how alkylating agents work, such as those used in chemotherapy. Nevertheless, MMS exerts additional actions, such as oxidation and acetylation of proteins. In this work, we introduce the important notion that MMS also triggers a lipid stress that stems from and affects the inner nuclear membrane. The inner nuclear membrane plays an essential role in virtually all genome stability maintenance pathways. Thus, we want to raise awareness that the relative contribution of lipid and genotoxic stresses when using MMS may be difficult to dissect and will matter in the conclusions drawn from those studies.     

GC-MS/SIM法测定盐酸鲁拉西酮片中甲磺酸酯类物质残留量

建立了气相色谱-质谱/选择离子监测法(GC-MS/SIM),检测盐酸鲁拉西酮片中甲磺酸酯类物质残留量。使用DB-624毛细管色谱柱(30m×0.32mm×1.8μm)实现了甲磺酸酯的分离,对提取溶剂、起始柱温、分流比等条件参数进行了优化。在选择离子监测模式(SIM)下,选取适宜的特征离子,进行定性定量分析。结果表明,目标物在0.01~0.40mg/L范围内线性关系均良好,线性相关系数(R2)均大于0.999;检出限、定量限均分别为0.003mg/L、0.01mg/L;在0.16、0.20、0.24mg/L三个加标浓度下,平均回收率为88.43%~104.15%,相对标准偏差为0.97%~1.82%。该方法精密度良好,操作简便快速、准确可靠、灵敏度高,适用于盐酸鲁拉西酮片中甲磺酸甲酯、甲磺酸乙酯和甲磺酸异丙酯残留的同时检测。