氯乙酸碱性水解法合成羟基乙酸单体的研究

以氯乙酸和氢氧化钠为主要原料,碘化钠为催化剂碱性水解法合成羟基乙酸,并采用单因素法对影响因素进行了研究,得到最优化条件:反应温度90℃,反应时间8 h,催化剂NaI用量为氯乙酸质量的0.8%。羟基乙酸的产率可达到73.1%。     

碘化钠催化合成l,4—二丁氧基苯的研究

以乙醇为溶剂 ,碘化钠为催化剂 ,由金属钠、对苯二酚和溴丁烷合成了 1 ,4 -二丁氧基苯。考察了影响收率的因素 ,最佳合成条件为 :物料溴丁烷 :对苯二酚 :金属钠 :碘化钠为 2 .5mol:1mol:2 .2mol:0 .1 3mol,反应在回流温度下进行 ,反应时间 2 .5小时 ,收率可达 90 .6 %。     

有机电化学法电解合成环氧丙烷

此法是利用氯化钠(或氯化钾、溴化钠、碘化钠)的水溶液,经电解生成氯气和氢氧化钠的原理,在阳极区通入丙烯,生成氯丙醇,在阴极区氯丙醇与氢氧化钠作用生成环氧丙烷。其反应如下:     

原位合成碘催化蔗糖制备5-羟甲基糠醛

着重研究以原位合成碘(即三氯化铬和碘化钠发生氧化还原反应产生的碘)为催化剂,蔗糖为原料制备羟甲基糠醛.考察了反应时间、反应温度、催化剂用量(以三氯化铬和碘化钠质量计)、蔗糖质量百分数对羟甲基糠醛收率的影响.得到以原位合成碘为催化剂的优化条件:时间45min、温度130℃、催化剂用量0.25g、蔗糖质量百分数8%.在此优...     

碘化钠催化合成1，4—二丁氧基苯的研究

以乙醇为溶剂，碘化钠为催化剂，由金属钠、对苯二酚和溴丁烷合成了1，4-二丁氧基苯。考察了影响收率的因素，最佳合成条件为：物料溴丁烷：对苯二酚：金属钠：碘化钠为2.5mol:1mol:2.2mol:0.13mol，反应在回流温度下进行，反应时间2.5小时，收率可达90.6%。     

碘化钠催化合成1,4-二乙氧基苯的研究

以乙醇为溶剂，碘化钠为催化剂，由金属钠，对苯二酚和溴乙烷合成了1，4－二乙氧基苯，考察了影响收率的因素，最佳合成条件为：物料溴乙烷：对苯二酚：金属钠：碘化钠（摩尔比）为2．5：1：2．2：0．13，反应在回流温度下进行，反应时间2h，收率可达92．8％。     

膨润土深加工制备P型沸石

以廉价的膨润土为原料,分别进行了氢氧化钠水溶液高温活化和氢氧化钠碱熔活化制备P型沸石的实验,合成了两种结构不同的P型沸石,并对合成产品作了表征和物化性能测试.结果表明:碱法工艺具有资源利用率高,无废液排放等优点.合成的P型沸石性能比4A沸石优越,是理想的洗涤助剂替代品.     

对-正丁基苯胺合成过程中绿色催化剂的初选

以正丁醇和苯胺为反应物，分别选择碘化钠、碘化钾、碘的乙娉溶液为催化剂，在均相反应器中催化合成对-正丁基苯胺，产物用薄层层析色谱和气相色谱进行检测。结果表明：碘化钠、碘化钾、碘的乙醇溶液为催化剂时均可合成对-正丁基苯胺，其中以碘化钾作催化剂时的产率最高，达到25．63％。     

硬脂酸钕热稳定剂的改进复分解法合成研究

采用改进复合分解法合成硬脂酸钕,通过均匀设计实验,分析了反应温度、硝酸钕浓度、硬脂酸浓度、氢氧化钠浓度、氢氧化钠滴加时间、保温时间6个因素对合成反应的影响,确定较合适的合成工艺条件.采用电导率法测定硬脂酸钕对聚氯乙烯(PVC)的热稳定性能,结果表明硬脂酸钕热稳定性效果优异.     

常温合成条件对两步法制备氢氧化镁阻燃剂中试研究的影响

在自行研制的中试设备上用两步法（氢氧化钠合成法-水热反应法）制备出了氢氧化镁阻燃剂,分析了常温合成条件对制备氢氧化镁的影响.研究发现在相同的水热条件下,提高常温合成温度和降低氢氧化钠加料速率,有利于常温产物的水热改性处理,使之生成形貌规则、粒径分布均匀、分散性良好的氢氧化镁六方片状颗粒.     

Pronounced Catalytic Effect of Micellar Solution of Sodium Dodecyl Sulfate (SDS) for Regioselective Iodination of Aromatic Compounds with a Sodium Iodide/Cerium(IV) Trihydroxide Hydroperoxide System

Micellar solutions of sodium dodecyl sulfate (SDS) catalyze the regioselective iodination of a wide range of aromatic compounds with sodium iodide in the presence of the easily prepared, water‐resistant and recyclable cerium(IV) trihydroxide hydroperoxide, Ce(OH)₃O₂H, at room temperature. By this protocol, structurally diverse aromatic compounds including benzene and naphthalene were iodinated in good to excellent yields.     

Aerobic Oxidative Iodination of Organic Compounds with Iodide Catalyzed by Sodium Nitrite

Selective and efficient iodinations of organic compounds were achieved by an aerobic oxidative process catalyzed by sodium nitrite using potassium iodide in acidic media. Using the potasasium iodide (KI)/air/sodium nitrite (NaNO₂; cat.)/sulfuric acid (H₂SO₄) iodinating system, activated and moderately deactivated aromatic compounds were exclusively or preferentially iodinated at the para position. In protic solvents ketones and 1,3‐dicarbonyl compounds were iodofunctionalized at the α carbonyl position, while in the case of aryl methyl ketones bearing an activated aromatic ring, the regioselectivity of iodination could be directed by the solvent used. In acetonitrile (MeCN) the aromatic ring was selectively iodinated, while in aqueous rethanol (EtOH) functionalization of the methyl carbon atom took place. Alkenes were transformed to vicinal iodohydrins or vicinal iodoalkoxy derivatives following Markovnikov‐type regioselectivity and anti stereoselectivity, while 1,2‐diiodoalkenes with preferentially E orientation were formed from alkynes.     

三碘化铑的新合成方法

三氯化铑与氢碘酸直接合成碘化铑,在最佳反应条件下,合成的收率达到98.5%,产品晶形均一,氯离子含量小于50 mg/kg。     

Synthesis and Evaluation of 3,4‐Dihydropyrimidin‐2(1H)‐ones as Sodium Iodide Symporter Inhibitors

The sodium iodide symporter (NIS) is responsible for the accumulation of iodide in the thyroid gland. This transport process is involved in numerous thyroid dysfunctions and is the basis for human contamination in the case of exposure to radioactive iodine species. 4‐Aryl‐3,4‐dihydropyrimidin‐2(1H)‐ones were recently discovered by high‐throughput screening as the first NIS inhibitors. Described herein are the synthesis and evaluation of 115 derivatives with structural modifications at five key positions on the pyrimidone core. This study provides extensive structure–activity relationships for this new class of inhibitors that will serve as a basis for further development of compounds with in vivo efficacy and adequate pharmacokinetic properties. In addition, the SAR investigation provided a more potent compound, which exhibits an IC₅₀ value of 3.2 nM in a rat thyroid cell line (FRTL5).     

The Synthesis of (E)-Vinyl and Alkynyl Sulfones by the Formation of an Electron Donor-Acceptor Complex Using Thiosulfonates and Sodium Iodide Under Visible Light

A method for the synthesis of (E)-vinyl sulfones and alkynyl sulfones through the cleavage of thiosulfonate promoted by the formation of EDA complexes under visible light irradiation at room temperature without the need for other metal catalysts is described. The mechanism study shows that sodium iodide and thiosulfonate form EDA complexes under visible light irradiation, resulting in a single-electron transfer cleavage to generate sulfonyl radicals, which then react with olefins or alkynes to produce (E)-vinyl sulfones or alkynyl sulfones, respectively. This method is applicable to 44 olefin and alkyne substrates, with yields ranging from 38% to 90%, providing a radical synthesis approach for the preparation of sulfonylated compounds.     

Sodium Iodide/Hydrogen Peroxide‐Mediated Oxidation/Lactonization for the Construction of Spirocyclic Oxindole‐Lactones

The sodium iodide/hydrogen peroxide‐mediated oxidation/lactonization of indolepropionic acids was achieved, affording the corresponding spirocyclic oxindole‐lactones in moderate to high yields. This metal‐free procedure features mild reaction conditions, non‐toxicity and easy handling, with hydrogen peroxide (H₂O₂) as a clean oxidant.

     

三价铬对测定退铬溶液中氢氧化钠的影响

在氢氧化钠溶液中用电解法退铬,退镀液中产生亚铬酸钠。用酸碱滴定法以酚酞作指示剂测定氢氧化钠,亚铬酸钠影响测定结果。在生产过程中发现,用传统的酸碱滴定法测定氢氧化钠误差很大。通过实验改进了氢氧化钠的测定方法,用氯化钡沉淀亚铬酸钠等,以酚酞作指示剂,用盐酸滴定氢氧化钠的质量浓度。     

芒硝型卤水中盐硝组分对碱法脱除钙镁的影响

采用＂烧碱-纯碱＂法,对芒硝型卤水中Ca^2＋和Mg^2＋的脱除进行了研究,在常温、两碱用量为理论用量、反应时间为30 min和陈化时间为60 min的条件下详细考察了卤水中氯化钠和硫酸钠含量的变化对Ca2＋和Mg2＋脱除效果的影响。结果表明,硫酸钠组分对Ca2＋的脱除效果影响较大,当硫酸钠含量在30 g/L以下时,Ca2＋脱除率在90%以上,硫酸钠浓度增加有利于Mg2＋的脱除,但影响不大。氯化钠组分对Ca2＋、Mg2＋脱除效果的影响相对较小,氯化钠含量增加,Ca2＋脱除率明显增加,而Mg2＋脱除率略有下降。     

电位滴定法测定工业烧碱中氢氧化钠和碳酸钠的含量

目前GB／T4348．1—2000测定工业用氢氧化钠中氢氧化钠和碳酸钠含量时,采用的是化学滴定法,但是此方法存在耗时耗试剂等一系列缺点,不符合现代分析化学发展的趋势,而自动电位滴定法操作方便,测定快速准确,有利于实现化学分析的自动化。本实验用瑞士Metrohm682电位滴定仪对大量样品进行测定,数据表明,电位滴定法的准确度和精密度可以满足国标的要求,可用自动电位滴定法代替化学滴定法。