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氯苯丁酯

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After esterification, the ethyl-2-chloro-3-phenylpropionate reacts with diethyl malonate under the catalysis of sodium ethylate, and we obtain the corresponding triethyl ester. The-benzylsuccinic acid is formed by the triethyl ester reacting with concentrate hydrochloric acid and taking place hydrolyzation and decarboxylation reaction at the same time. In order to avoid the formation of cinnamic acid, the sodium ethylate and diethyl malonate must be react sufficiently. The course has simple operation, inexpensive materials and better yield.

具体制备工艺为:首先以L-苯丙氨酸为原料采用重氮化方法得到-2-氯-3-苯基丙酸,再经酯化得到-2-氯-3-苯基丙酸乙酯后在乙醇钠催化作用下和丙二酸二乙酯缩合,发生SN2反应,得到相应的三乙酯,然后经水解和脱羧,得到-苄基丁二酸;在实验中乙醇钠要和丙二酸二乙酯充分反应,避免生成肉桂酸乙酯;该过程操作简单,原料便宜,产率较高,总收率可达到26.8%。

During the manufacturing of the critical intermediate cephalosporin nucleus --7-amino-3-chloro-cephalosporanic acid diphenylmethyl ester hydrochloride salt, first the feasibility of the one-pot synthetic route of open loop, closed loop and ozonization when chlorine is passed over is qualified by experiments. Then the critical factors that will influence this reaction are studied as follows: the mol ratio of triphenyl phosphite and Diphenylmethyl 3-hydroxy-7-phenylacetaminoceph-3-em-4-carboxylate-l-oxide is four to one; the quantity of the stablizer should be at least more than two to one. The temperature of the system must be 25℃ when chlorine is passed over so that the hydrochloride can be precipitated to obtain cephalosporin nucleus of cefaclor--7-amino-3-chloro-cephalosporanic acid diphenylmethyl ester hydrochloride salt.

在制备关键中间体头孢母核7-氨基-3-氯头孢烷酸二苯甲酯盐酸盐时,先通过实验验证把开环、闭环、臭氧化三步在通入氯气时并为一锅煮的合成路线的可行性之外,又研究了影响该反应的几个重要因素:亚磷酸三苯酯与3-羟基-7-头孢烷-5-亚砜-2-甲酸二苯甲酯的摩尔比为4:1;稳定剂2-甲基-2-丁烯的用量至少大于2:1,通入氯化氢气体时体系温度在25℃时盐酸盐则能够顺利析出,获得头孢克洛的头孢母核—7-氨基-3-氯头孢烷酸二苯甲酯盐酸盐。

The optimal carrier gas velocity of prepared SE-30 series capillary chromatographic columns was studied and used to separate isomeric compounds. The efficiency of SE-30 capillary chromatographic columns has been studied with different diameters, film thicknesses and oven temperatures, using n-do-decane, phenol, aminobenzene, and butyl acetate as test samples.

研究自制的SE-30系列毛细管气相色谱柱的载气最佳线速度,并应用于同分异构体的色谱分离分别用十二烷、苯酚、苯胺、醋酸丁酯作试祥在不同载气线速条件下对不同口径、不同膜厚、不同柱温的SE-30毛细管色谱柱的柱效进行考察,并在最佳线速度条件下分离异戊醇、硝基氯苯、硝基甲苯及二乙苯同分异构体体系。

The main products are: phosphorous trichloride 300,000 tons / year, phosphorus oxychloride 100,000 tons / year, phosphorus pentachloride 50,000 tons / year, 10,000 tons trichloroisocyanuric parathion / year chloromethyl ether 5000 tons / year, triethyl phosphite 10,000 tons / year, triphenyl phosphite 5000 tons / year, three phosphoric acid ethyl butoxy 2000 tons / year.

主要产品有:三氯化磷30万吨/年、三氯氧磷10万吨/年、五氯化磷5万吨/年、三氯硫磷1万吨/年、氯甲基甲醚5000吨/年、磷酸三乙酯10000吨/年、磷酸三苯酯5000吨/年、磷酸三丁氧基乙酯2000吨/年。

Our company supply raw materials and related intermediates as follows: Second dibutyryl cAMP calcium, voriconazole, terbinafine, vecuronium amines, cAMP, thiamphenicol, a chlorophenol hydrochloride esters, card network sodium phosphate tilmicosin, foscarnet, lornoxicam, Tilmicosin, Cephalosporium aspirin acid, ceftiofur hydrochloride, ceftiofur sodium, Ozagrel, ondansetron hydrochloride ketones, hydroxyurea, ticarcillin sodium, telmisartan, esmolol hydrochloride, hydrochloric acid Daguan Nikkomycin, adefovir dipivoxil, buflomedil hydrochloride, granisetron hydrochloride, warfarin sodium,-methyl gabexate acid, nicergoline, pantoprazole sodium,·, tegafur, cefepime hydrochloride, vecuronium bromide, hydrochloric acid meclofenoxate, sertraline hydrochloride, Cefonicid amine salt, aztreonam, ticarcillin, cefdinir, cefodizime sodium, sodium ferulate, colloidal pectin secretion, 2,3 - cyclopentene and pyridine, Piperacillin acid, cefetamet US-acid, hydrochloride Cefmenoxime ,3-TZ, 2 - deoxy-D-glucose, two-amidine urea benzene, sodium Cefonicid, Cefonicid intermediates, ester Cefamandole sodium, Cefalotin acid, intermediates cefpirome, cefepime sulphate, cefepime intermediate nucleus of cefepime, cefpirome nucleus, Cefamandole sodium, ceftriaxone new active ester, oxaliplatin, cyclophosphamide vary gland amines, polyene match him.

我公司供应的原料药及相关中间体为:二丁酰环磷腺苷钙、伏立康唑、盐酸特比萘芬、维库溴胺、环磷腺苷、甲砜霉素、盐酸甲氯酚酯、卡络磺钠、磷酸替米考星、膦甲酸钠、氯诺昔康、替米考星、头孢匹胺酸、头孢噻呋盐酸盐、头孢噻呋钠、奥扎格雷、盐酸恩丹西酮、羟基脲、替卡西林钠、替米沙坦、盐酸艾司洛尔、盐酸大观霉素、阿德福韦酯、盐酸丁咯地尔、盐酸格拉司琼、华法林钠、甲磺酸加贝酯、尼麦角林、泮托拉唑钠、普拉洛芬、替加氟、盐酸头孢吡肟、维库溴铵、盐酸甲氯芬酯、盐酸舍曲林、头孢尼西胺盐、氨曲南、替卡西林、头孢地尼、头孢地嗪钠、阿魏酸钠、胶体果胶泌、2,3-环戊烯并吡啶、哌拉西林酸、头孢他美酸、头孢甲肟盐酸盐、3-TZ、2-脱氧-D-葡萄糖、双脒苯脲、头孢尼西钠、头孢尼西中间体、头孢孟多酯钠、头孢噻吩酸、头孢匹罗中间体、头孢吡肟硫酸盐、头孢吡肟中间体、头孢吡肟母核、头孢匹罗母核、头孢孟多钠、头孢曲松新型活性酯、奥沙利铂、异环磷腺胺,多烯他赛。

The famciclovir was synthesized from purine by a series of steps by Acylation, Decarboxylation, Reduction ,and so on; Derivatives of these intermediates is described from the 6-chloro- 9H- purin-2-amine as raw materials in different conditions when the iodine and bromide were synthesized with the addition of two intermediate 6-bromo-9H-purin-2-amine and 6-iodo-9H-purin-2-amine; There is elaborated from the main part of a acetophenone, urineaminohydrochloride, phenylhydrazine, ethyl acetoacetate as raw material through a series of reactions to synthetic 3-phenyl-4-formylphenyl pyrazole and 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-aldehyde two pyrazole aldehyde, and then with 2-amino-6-chlorine-9-(2-methicillin-oxo-co-methyl-4-yl) purine reaction of the two new pyrazole purine Schiff bases.

本论文主是采用以鸟嘌呤为原料,经过一系列的酰基化,脱羧,还原等反应作用下最终得到了产物2-氨基-9-(4-乙酰氧基-3-乙酰氧基甲基丁基)嘌呤;其中的中间体衍生物主要是阐述从以2-氨基-6-氯鸟嘌呤为原料通过在不同的条件下进行溴代与碘代分别合成了另外两种中间体2-氨基-6-溴鸟嘌呤及2-氨基-6-碘鸟嘌呤;还有一部分主要是阐述从以苯乙酮,盐酸氨基脲,苯肼,乙酰乙酸乙酯为原料通过一系列的反应先合成3-苯基-4-醛基吡唑及5-氯-3-甲基-1-苯基-1H-吡唑-4-甲醛这两个吡唑醛,然后再与2-氨基-6-氯-9-(2-甲氧羰基丁酸甲酯-4-基)嘌呤反应得到了两个新型的吡唑嘌呤席夫碱

In this study, new benzo[l,2,3]thiadiazole derivatives were designed according to relationship of structure and efficacy. The 9 novel compounds were synsthesized with following reactions. The chlorine atom in 2-chloro-3,5-dinitro-benzoic acid as beginning raw material was substituted by 2-methylpropane-2-thiol, esterified then with bromoethane, reduced by iron powder and cyclized to obtain ethyl benzo[l,2,3]thiadiazole-7 after diazonation reation.

本论文根据苯并噻二唑诱导剂的构效关系设计了新的苯并噻二唑的结构,并合成了9个未见文献报道的化合物,合成步骤如下:采用2-氯-3,5-二硝基苯甲酸为起始原料,苯环上的氯原子被叔丁基硫醇置换,羧酸由溴乙烷酯化,硝基由铁粉还原,随后经重氮化关环生成苯并[1,2,3]噻二唑-7-羧酸乙酯。

Chloroacetic acid,chloromethyl ether,acetone,mphenylenediamine,butyl acetate,ethyl acetate,methylene chloride,ethylene dichloride,dioxane.

氯乙酸,氯甲醚,丙酮,间苯二胺,醋酸丁酯,醋酸乙酯,二氯甲烷,二氯乙烷,二氧六环。

These tests showed pu-erh performed at least as well as clofibrate, the most advanced medicine for the purpose, without the drug's side effects.

这些试验表明普洱茶在这方面的功效不差于专门用于治疗高血脂的药物--对氯苯氧异丁酸乙酯,而且没有这种药物的副作用。

The major occupational hazards factors in printing ink were benzene, toluene, xylene, ethylbenzene, solvent gasoline, methanol, alcohol, isopropyl alcohol, ethyl acetate, butyl acetate, butyl acetate, dichloromethane, etc. 10 of 1224 samples (0.82%) exceeded the national occupational health standards.

印刷油墨中存在的职业病危害因素种类主要有苯、甲苯、二甲苯、乙苯、溶剂汽油、甲醇、乙醇、异丙醇、乙酸乙酯、乙酸丁酯、二氯甲烷等,检测样品总数1224件,超标样品数10件,超标率为0.82%。

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