溶剂法合成2—羟基—3—萘甲酸技术的进展

介绍了办内外溶剂法生产２－羟基－３－萘甲酸的进展珠况，并推茂采溶剂法规模化生产２－羟基－３－萘甲酸。     

溶剂法合成2-羟基-3-萘甲酸技术进展

介绍了国内外溶剂法生产２－羟基－３－萘甲酸的进展情况,并推荐采用溶剂法规模化生产２－羟基－３－萘甲酸     

2-羟基-3-萘甲酸生产新工艺开发成功

由沈阳化工研究院沈阳精细化工技术研究推广中心开发的溶剂法合成２－羟基－３－萘甲酸新工艺获得成功。２－羟基－３－萘甲酸是制造冰染染料和有机颜料的重要有机中间体。国内自５０年代以来，一直采用气、固相法生产，在工艺、设备、产品质量、原料消耗和环境保护等方面都存在不少问题。江苏省靖江溶剂厂采用新工艺，投资建成年产１０００ｔ２－羟基－３－萘甲酸装置，新工艺对反应器结构无特殊要求，工艺中有机溶剂的选择、羟化反应的工艺条件及后处理方法等具有一定的独创性，达到９０年代国际先进水平。2-羟基-3-萘甲酸生产新工艺开发…     

合成1,4—二羟基—2—萘甲酸方法的改进

１，４－二羟基－２－萘甲酸以改进的Ｈｏｍｅｇｅｒ法进行制备，具有操作方便，溶剂耗费少，不使用苯及乙醚的萃取步骤，总反应时间也缩短到原来的１／４，而且产品纯度和产率都有提高。改进后的方法用于大规模工业生产将产生较好的经济效益。     

以甲苯为溶剂合成2-羟基-1-萘甲酸的新工艺

介绍了一种以甲苯为溶剂合成２－羟基－１－萘甲酸的新工艺。将β－萘酚溶解于甲苯溶剂中,与ＮａＯＨ溶液混合加热生成β－萘酚钠盐,再于９０～１２０℃、０．４～２ＭＰａ压力下通入ＣＯ２,产品收率可达７０％。     

水相催化法制备1－苯基－3－羟基－1，2，4－三唑

水相催化法制备１－苯基－３－羟基－１，２，４－三唑汪传木（安徽省池州农药厂，２４７１００）１－苯基－３－羟基－１．２．４－三唑（以下简称苯唑醇）是合成新型杀虫杀螨剂三唑磷的重要中间体。目前，国内生产三唑磷的厂家较多，均采用溶剂法制备苯唑醇，该方法制备...     

合成1，4－二羟基－2－萘甲酸方法的改进

１，４－二羟基－２－萘甲酸以改进的Ｈｏｍｅｇｅｒ法进行制备，具有操作方便，溶剂耗费少，不使用苯及乙醇的萃取步骤，总反应时间也缩短到原来的１／４，而且产品纯度和产率都有提高。改进后的方法用于大规模工业生产将产生较好的经济效益。     

高效液相色谱测定2－羟基－3－萘甲酸中2－萘酚含量

采用μ－ＢｏｎｄａｐａｋＣ（１８）固定相、甲醇／水（９０／１０）和０．５ｍｏｌ／ＬＮａ２ＨＰＯ４流动相，３００ｎｍ检测波长和１．２ｍｌ／ｍｉｎ流速，对２－羟基－３－萘甲酸中小量２－萘酚进行高效液相色谱测定，取得了较满意的结果。     

N,N—双（2—羟基乙基）—N—（3—十二烷氧基—2—羟丙基）甲铵硫酸甲酯盐含量的测定

介绍了Ｎ，Ｎ－双（２－羟基乙基）－Ｎ－（３－十二烷氧基－２－羟丙基）甲铵硫酸酯盐的定量分析方法，该法操作简便，分析结果准确，为生产和应用该表面活性剂的厂家提供了可靠的分析手段。     

3—硝基—N—乙基咔唑单溴化反应的研究

研究了在不同的溶剂和后处理方式下３－硝基－Ｎ－乙基中文唑单溴化的三种方法：（１）冰醋酸－水稀释法；（２）冰醋酸－蒸馏法；（３）１，２－二氯乙烷－蒸馏法。比较了三种方法各自的优缺点，认为（３）法是较佳的工业化路线。     

环虫酰肼的合成

乙酰乙酸乙酯与甲醛缩合,然后脱羧得到2-甲基-4-氧-2-环己烯甲酸乙酯,在四乙基溴化铵催化下与1-溴-3-氯丙烷反应,得到5-甲基-7,8-2H-6-苯并二氢吡喃甲酸乙酯,再在硫粉的催化下脱氢得到5-甲基苯并二氢吡喃-6-甲酸乙酯,然后经水解、酰肼化得到关键中间体N-5-甲基苯并二氢吡喃-6-甲酰-N'-特丁基肼,最后与3,5-二甲基苯甲酰氯反应得到环虫酰肼,总收率23.3%。     

An efficient,clean synthesis of 3,3′-(arylmethylene)bis(2-hydroxynaphthalene-1,4-dione) derivatives

A clean, simple and efficient method for the synthesis of 3,3′-(arylmethylene)bis(2-hydroxynaphthalene-1,4-dione) derivatives has been developed which uses the reaction of 2-hydroxynaphthalene-1,4-dione and aromatic aldehydes in the presence of a catalytic amount of LiCl in aqueous media. To the best of our knowledge, this is the first report on such a synthesis of 3,3′-(arylmethylene)bis(2-hydroxynaphthalene-1,4-dione).     

Kinetic and thermodynamic studies of acid scarlet 3R adsorption onto low-cost adsorbent developed from sludge and straw简

A low-cost adsorbent was prepared from sludge and straw by pyrolysis in a dried state with the surface area of the adsorbent of 829.49 ma. g-l, micropore volume of 0.176 cm2·g-1 and average pore radius of 5.0 nm. The kinetic, equilibrium isotherm and thermodynamic characteristics of trisodium 1-（1-naphthylazo）-2-hydroxynaphthalene- 4＇,6,8-trisulphonate （acid scarlet 3R） onto the adsorbent from sludge and straw were investigated. The results indicated that the pseudo second order adsorption was the predominant adsorption mechanism of acid scarlet 3R. Thus, the adsorption phenomenon was suggested as a chemical process. The adsorption data were fitted better with Langmuir model than Freundlich model, indicating that the adsorption of acid scarlet 3R belonged to the monolayer adsorption and mainly occurred in micropores.     

One-Pot,Sequential Four-Component Synthesis of Benzo[a]chromeno[2,3-c]phenazine Derivatives Using SiO2–SO3H as an Efficient and Recoverable Catalyst Under Conventional Heating and Microwave Irradiation

Silica sulfuric acid (SiO₂–SO₃H) has been used as an effective and reusable solid catalyst for the one-pot, two-step, four-component microwave-assisted synthesis of benzo[a]chromeno[2,3-c]phenazine derivatives by the condensation reaction of 2-hydroxynaphthalene-1,4-dione, o-phenylenediamine, aldehydes, and cyclic 1,3-dicarbonyl compounds. This new procedure has a number of advantages such as: high yields, very short reaction time, operational simplicity, simple work-up procedures and avoidance of hazardous or toxic catalysts, and organic solvents and is devoid of inessential derivatization and generation of hazardous substances. Moreover, the catalyst shows high thermal stability and can be recovered and reused without loss of reactivity.     

The efficient synthesis of aryl-5H-dibenzo[b,i]xanthene-5,7,12,14(13H)-tetraone leuco-dye derivatives

An efficient method for the synthesis of 13-aryl-5H-dibenzo[b,i]xanthene-5,7,12,14(13H)-tetraone derivatives by the reaction of 2-hydroxynaphthalene-1,4-dione and aldehydes in the presence of a catalytic amount of p-toluene sulfonic acid under solvent-free conditions at 100 °C is described.     

6-羟基-2-萘磺酸铜、镁、锌、钴、镍配合物的合成和结构表征

6-羟基-2-萘磺酸钠分别和CuSO4,MgSO4,ZnSO4、Co(phen)3Cl2反应,物质的量比为5∶1,得到一系列铜、镁、锌、钴、镍配合物并通过红外和元素分析确定结构。测定了钴的配合物的单晶结构,结果表明,钴配合物1属于三斜晶系,P-1空间群,a=12.4120(15),b=12.4711(16),c=20.090(2),α=90.0450(10)°,β=103.161(2)°,γ=113.519(2)°,V=2761.9(6)3,Z=2。     

一种头孢丙烯一水合物的制备方法

以7-氨基-3-((Z/E)-丙烯-1-基)-3-头孢烯-4-羧酸(7-APCA)和D-对羟基苯甘氨酸邓钾盐(简称"羟邓盐")为起始原料,经混酐、成盐及缩合反应后,得到头孢丙烯N,N-二甲基甲酰胺(DMF)溶剂化物,之后用水将DMF置换,得到头孢丙烯一水合物。在缩合反应进行期间,加入N,N-二甲基苯胺调节体系pH,使得随后的缩合更容易进行,缩短了反应时间,提高了收率。     

Express method of the quantitative determination of nitrites by computer colorimetry using new reagent compositions

The possibilities of using new reagent compositions based on diazo and azo dyestuff components that contain sulfonic groups are considered to determine nitrites in the presence of the contents of chlorides. New reagent compositions based on 1-hydroxynaphthalene-3,6-disulfonic acid in combination with 2,6- nitroorthanilic and 2,6-dichlorosulfanilic acids have been used to create indicator powders and indicator papers for the quantitative test determination of nitrite ions. Test methods based on sustainable indicator powders and indicator papers have been developed with the use of the ilPro portable spectrophotometer and PlustekSmartPhoto P60 compact mobile scanner combined with the Vuescan universal scan program. It has been shown that the sensitivity of the visual determination of nitrites in liquids using indicator papers is 0.5 mg/L. The sensitivity of the test method that uses indicator papers, the PlustekSmartPhoto P60 mobile scanner, and the ilPro portable spectrophotometer is 0.2 mg/L. Upon using the indicator powder and i1Pro portable spectrophotometer, the range of defined concentrations of nitrite ions is 0.01–5 mg/L.     

氯虫苯甲酰胺的合成及表征

以3-甲基-2-硝基苯甲酸为原料通过RaneyNi加氢还原制得3-甲基-2-氨基苯甲酸,接着与N-氯代丁二酰亚胺(NCS)反应制得3-甲基-2-氨基-5-氯苯甲酸,然后3-甲基-2-氨基-5-氯苯甲酸与氯化亚砜在75～80℃下回流3h后,接着缓慢滴加甲胺水溶液,在室温下搅拌反应12h,得到2-氨基-5-氯-N,3-二甲基甲酰胺。然后再与3-溴-1-(3-氯吡啶-2-吡啶基)-1 H-吡唑-5-甲酸在-5～0℃下滴加甲基磺酰氯反应得到产品氯虫苯甲酰胺,四步总收率37.0%,产品HPLC纯度是96.05%。     

Zn~(2+)-Ni~(2+)-Fe~(3+)-LDHs新型催化剂的制备及其酸性研究

以Ni(NO3)2?6H2O、Zn(NO3)2?6H2O、Fe Cl3?6H2O为原料,采用均相沉淀法制备了层状形貌的Zn~(2+)-Ni~(2+)-Fe~(3+)-LDHs催化剂材料。吡啶作为分子探针,通过原位红外技术对Zn~(2+)-Ni~(2+)-Fe~(3+)-LDHs的酸性中心和酸量进行了研究。研究表明该材料同时存在路易斯酸(L酸)和布朗克(B酸)酸性中心,其酸量分别为4.4 mmol/g、2.6 mmol/g,L酸酸强度强B于酸。