苯乙腈

Methods 4-Hydroxy- benzonitrile was treated with sodium hydrogen sulfide and anhydrous magnesium chloride in dimethyl formamide to give thioamide, which was then directly cyclized with ethyl 2-chloroacetoacetate without separation to give ethyl 2-(4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(2) in one-pot; then 2 was formylated with Duff reaction adopting hexamethylenetetramine in trifluoroacetic acid to give ethyl 2-(3-formyl-4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(3); finally, the target compound was obtained by the treatment of 3 with hydroxylamine hydrochloride and sodium formate in formic acid.

采用"一勺烩"方法，以4-羟基苯甲腈为起始原料，首先与硫氢化钠和无水氯化镁在N，N-二甲基甲酰胺中反应，所得中间体不经分离，直接加入2-氯乙酰乙酸乙酯进行环合反应，得到2-(4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯（2）；然后通过六亚甲基四胺/三氟乙酸进行Duff反应，得到2-(3-甲酰基-4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯（3）；再经盐酸羟胺/甲酸/甲酸钠体系脱水得到目标化合物。

Three ways leads to the synthesis of fenclorin, one way discussed here has 3 steps. Stepl :benzonitrile using as raw material goes though dry hydrogen chloride and becomes a-imino phenylmethyl ether after meet carbinol.

解草啶的合成主要有三条路线，本文选取合成路线是以苯甲腈为原料，经三步反应而成：1、苯甲腈在干燥的氯化氢通入，与甲醇形成亚氨基苯甲醚，通入氨气后置换甲氧基得到苯基脒盐酸盐(收率76.18%)。2、苯基脒盐酸盐在碱性条件下与丙二酸二乙酯环合而得嘧啶醇(收率84.39%)。3、嘧啶醇在三氯氧磷中羟基被氯化得到产品解草啶(收率87.29%)。

Methods: Glipizide gliclazide glyburide glimepiride gliquidone repaglinide nateglinide pioglitazone rosiglitazone metformin phenformin and tolbutamide added in the blank ground samples were extracted with 80% methanol and were separated from an ACQUITY UPLC DBH C18 column with a gradient mobile phase of acetonitrile - 0.2 % formic acid water solution. A tandem quadrupole mass spectrometer equipped with electrospray ionization source was used in positive ion mode multiple reaction monitoring was performed to quantify above mentioned compounds.

被添加在中成药制剂及其包装物中的二甲双胍、苯乙双胍、罗格列酮、吡格列酮、格列吡嗫娶瑞格列奈、甲苯磺丁脲、格列齐特、格列苯脲、那格列奈、格列美脲、格列喹酮等西药成分用80%甲醇提取，以乙腈- 0.2%甲酸水溶液为流动相梯度洗脱，在ACQUITY UPLC DBH C18色谱柱上分离，串联四级杆质谱检测，MRM方式采集并定量。

A series of N -bonded donor-acceptor derivatives of phenothiazine containing phenyl, anisyl, pyridyl, naphthyl, acetylphenyl, and cyanophenyl as an electron acceptor have been synthesized.

合成了一系列的N10位取代的吩噻嗪给体受体衍生物，这些受体基团包括苯，苯甲醚，吡啶，萘，苯乙酮和苯甲腈。

Computationalresults indicate that the no-planar trans-benzanilide is the most stable structure. The spectra indicate that the Franck Condon region photodissociation dynamics have multidimensional character withnine activemodes. The intensity of υ24 mode in methanol is much stronger than that in acetonitrile. Compared with fatty amides and benzamide, phenyl substitution for H atom on-NH2 group makes C=O solvent effects disappear.

结果表明，苯甲酰苯胺的非平面反式结构为最稳定结构；在Frank-Condon区域内，苯甲酰苯胺主要由9个活性振动模组成；其中ν24（苯环上C＝C不对称伸缩振动和CCH的面内弯曲振动，NH面内弯曲振动）振动模在甲醇溶剂中的强度远远大于其在乙腈的强度；与脂肪酰胺类化合物和苯甲酰胺的研究结果比较发现，苯基取代－NH2上的H原子使得C＝O不再具有明显的溶剂效应。

Methods: In alkaline condition, reaction between amino acids and phenylisothiocyanate formed a derivant of phenylisothiocyanate-amino acid. For RP-HPLC, the Diamonsil C18 column 250 mm×4.6 mm,5 μm） and binary gradient elution were used. The mobile phase A was 0.1 mol/L sodium acetate solution-acetonitrile (93∶7） and the mobile phase B was acetonitrile-water（80∶20）. The detecting wavelength was 254 nm.

在碱性条件下，氨基酸与异硫氰酸苯酯反应，生成异硫氰酸苯–氨基酸的衍生物，采用 Diamonsil C18色谱柱（250 mm×4.6 mm，5 μm），用二元梯度洗脱方式，流动相A为0.1 mol/L乙酸钠–乙腈（93∶7），流动相B为乙腈–水（80∶20），检测波长254 nm。

The first synthetic route uses 1,2,4-trimethoxybenzene and chloroacetonitrile in forming 2,4,5-trimethoxy-a-chlor-acetophenone under the anhydrous condition, then the intermediate condensates with papaverine forming the core pyrro[2,l-a]isoquinoline, followed by formation and lactonization to form the lactone ring. The second synthetic route uses prepared aldehyde with prepared ethyl nitroacetate by Knoevenagel condensation to obtain 2-Nitro-3-(2,4,5-tris-methoxy-phenyl)-acrylic acid ethyl ester and 2-Nitro-3-(2,4,5-tris-benzyloxy -phenyl)-acrylic acid ethyl ester etal intermediates. The lamellarin skeleton could arise from condensation of the papaverine and these intermediates by Michael reaction, the ester group is provided for subsequent lactonization. The third synthetic route uses coumarin or indan-l,3-dione derivatives and papaverine to form lamellarin under basic conditions.

第一条路线首先从1，2，4-三甲氧基苯出发与卤乙腈作用合成卤代芳酮中间体，然后与罂粟碱反应合成开链片螺素，最后经乙酰化、去保护、成内酯环得到片螺素；第二条路线由制备的芳醛和制备的硝基乙酸乙酯经缩合得到2-硝基-3-芳基丙烯酸乙酯，然后由该中间体与罂粟碱反应，在完成关环的同时也引入酯基，最后去保护、成内酯环得到片螺素；第三条路线是由香豆素或茚二酮出发，经溴代后的中间体与罂粟碱反应，得到片螺素的基本框架。

Mm, 5 μm and a UV detector. Elution was performed at a flow rate of 1 mL/min, with a gradient of methanol-acetonitrile-water starting at 80∶10∶10, increasing linearly to 86∶10∶4 in 35 min, then returning to the initial conditions in 5 min. Elution of phenacyl esters was monitored by absorbance at 254 nm. Pentadecanoic acid was used to be an internal standard.

分析所用色谱柱为ZORBAXSB C18柱，以十七酸作为内标，甲醇-乙腈-水为流动相，采用梯度洗脱(梯度洗脱程序为甲醇-乙腈-水由80∶10∶10在35 min内线性变化到86∶10∶4，然后在5 min内恢复到起始比例，流动相流速为1 mL/min)，通过测定苯乙酰甲酯在254 nm处的吸光度值来测定脂肪酸含量。

By using isopropyl benzene as the internal standard material, using Agilent 1100 HPLC, using methanol-acetonitrile-water as mobile phase ,using three-component grade elution program, the components that contain benzene such as TALD,PT,4-CBA,TA,BA,PX and internal standard material isopropyl benzene in liquid phase product was analysed. Shimazu6A GC was used to analyse the solvent acetic acid and internal standard material isopropyl benzne in liquid phase.

以异丙苯为内标物，应用Agilent1100高效液相色谱仪，用甲醇－乙腈－水为流动相，采用三元梯度洗脱程序分析液相产物中的含苯环组分对甲基苯甲醛、对甲基苯甲酸、对羧基苯甲醛、对苯二甲酸、苯甲酸、对二甲苯和内标物异丙苯，应用Shimazu6A气相色谱仪分析液相中的溶剂醋酸和内标物异丙苯。

OBJECTIVE:To establish the RP-HPLC method for determination of methyl hydroxybenzoate and ethyl hydroxybenzoate in oral liquid preparations METHODS:The Nova-Park C18 column(3 9mm×150mm,5μm)was used The mobile phase consisted of acetonitrile-water(25∶75)at a flow rate of 1ml/min,the detection wavelength was set at 254nm and the sensitivity was set at 0 01 AUFS RESULTS:The linear ranges of methyl hydroxybenzoate and ethyl hydroxybenzoate were 0 4 412～13 2 360μg/ml(r=0 9 999) and 0 6 672～20 0 160μg/m...

目的 ：建立内服液体制剂中羟苯甲酯和羟苯乙酯的反相高效液相色谱测定方法。方法：色谱柱：Nova -ParkC18 柱(3 9mm×150mm ，5μm)；流动相：乙腈-水(25∶75)；流速：1ml/min ；检测波长：254nm ；灵敏度：0 01AUFS。结果：羟苯甲酯浓度在0 4412～13 2360μg/ml范围内线性关系良好(r=0 9999)；羟苯乙酯浓度在0 6672～20 0160μg/ml范围内线性关系良好(r=0 9998)。结论：该方法简便、快速、准确，可用于医院制剂中防腐剂的检测。

Now, however, all children continue in "comprehensive" schools, and the eleven-plus determines which courses of study the child will follow.

然而现在，所有的孩子都要在综合学校继续学习，所以这次考试只是决定他们将要学习哪些课程。

Cultivatable land , and led to a general recognition that development must not be carried at the cost of agriculture .

城区的迅速扩大在很多情况下侵占了宝贵的可耕地，使人们普遍认识到发展不能以牺牲农业为代价。