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甲酰化

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The optimum reaction conditions are as follows: diphenylmethanethiol : methyl chloroacetate is 1:1.5, and the reaction carried out at 100℃ for 4 h, 2- acetamide can be carried out in the room temperature for 20 h, the yield of 2- acetamide was 76%, hydrogen dioxide: 2- acetamide is 1:1, and the reaction carried out at 60℃ for 3 h, the yield of modafinil was 79%, the total yield of reaction can be reached 48%.

研究表明,采用氯乙酸甲酯作为醚化试剂,反应时间4h,反应温度100℃,二苯甲硫醇:氯乙酸甲酯=1:1.5,室温下氨解反应20h,二苯甲硫乙酰胺收率76%;采用过氧化氢作为氧化试剂,反应时间3h,反应温度60℃,过氧化氢:二苯甲硫乙酰胺=1:l,莫达非尼收率79%,反应总收率可达48%。

Nitro-4-methylsulfonylbenzoic acid was prepared from 4-toluene sulfonyl chloride by the reaction of Alkylation (in the condition of sodium sulfite and baking soda), Nitrification (in the condition of nitric acid and vitriol) and Oxidation reaction (in the condition of nitric acid and catalyzer).

研究了以对甲苯磺酰氯为起始原料,首先通过亚硫酸钠和碳酸氢钠的水溶液进行烷基化、其次在浓硝酸和浓硫酸加热回流的条件下峭化、最后在浓硝酸和催化剂的条件下进行氧化,3步反应合成了玉米田高效除草剂甲基磺草酮的重要中间体2-硝基-4-甲磺酰基苯甲酸。

This work, concentrated on the asymmetric allylation of aldehydes controlled by different chiral auxiliaries prepared from rotational pure tartaric acid, can be divided into three parts.The first part aims to review the developments of chiral drugs and asymmetric synthesis, from which derived the present research topic backgrounds and works.Synthesis and applications of allylation from aldehydes are the second part of the thesis. By optimizing the reaction conditions, such as solvents, temperature, time and chiral auxiliaries like N,N\'-dibenzyl tartamide, N,N\'-p-dimethylphenyl tartamide, N,N\'-o-dimethylphenyl tartamide, N,N\'-o-dichlorophenyl tartamide, N,N\'-a-dinaphyl tartamide, N,N\'-dicyclohexyl tartamide and N,N\'-diphenyl tartamide, ideal experimenttal conditions are obtained according to HPLC monitoring, as well as the auxiliaries\' recoveries experiments. Starting from benzaldehyde and 3-bromopropaldehyde, N,N\'-dibenzyl tartamide is considered the best auxiliary in this reaction.

本文介绍了醛的不对称烯丙基化反应,以光学纯酒石酸为原料,研究了不同构型手性配体在醛的烯丙基化反应中的立体选择性,全文共分三部分十个章节:第一部分对当前手性药物和手性技术进行了概述,并由此展开了本文的研究背景和任务;第二部分为有机合成部分,对醛的不对称烯丙基化反应进行了深入探讨,以苯甲醛为原料对反应条件进行优化,在优化的反应条件下对制备的七种可回收手性酰胺配体(N-苄基酒石酸二酰胺、N-对甲苯基酒石酸二酰胺、N-邻甲苯基酒石酸二酰胺、N-邻氯苯基酒石酸二酰胺、N-a-萘基酒石酸二酰胺、N-环己基酒石酸二酰胺和N-苯基酒石酸二酰胺)进行筛选,优化配体回收实验条件,最终确定出N-苄基酒石酸二酰胺在苯甲醛的不对称烯丙基化反应中具有较大优越性,结晶回收的手性配体光学纯度保持不变。

Water, Sodium Laureth Sulfate, Cocamidopropyl Betaine, Cocamide MEA, Disodium Cocamphodiacetate, Sodium Lauryl Sulfate, PEG 40 Hydrogenated Castor Oil, Perfume, Sodium Chloride, Propylene Glycol, Quaternium 80, Methylparaben, Polyquaternium 10, Hydroxypropyl Guar Hydroxpropyltrimonium Chloride, Citric Acid, Diazolidinyl Urea, Tetrasodium EDTA, Polyquaternium 7, Propylparaben, Sodium Hydroxide, Panthenol, Persea Gratissima Oil, Penta Sodium Pentetate, Hedera Helix Extract, Bambusa Vulgaris Extract

水,月桂醇聚醚硫酸酯钠,椰油酰胺丙基甜菜碱,椰油酰胺MEA,椰油酰两性基二乙酸二钠,月桂醇硫酸酯钠,PEG 40 氢化篦麻油,香料,氯化钠,丙二醇,季铵盐-80,苯甲酸甲脂,聚季铵盐-10,羟丙基瓜尔胶羟丙基三甲基氯化铵,柠檬酸,重氮烷基咪唑脲,乙二氨四醋酸四钠,聚季铵盐-7,对羟基苯甲酸丙酯,氢氧化钠,泛酰醇,酪梨油,喷替酸五钠,常春藤萃取物,银竹萃取物。

The α-monobromination of 2-pentone,4-methyl acetophenone,4-methoxyacetophenone,6-methoxy-2-acetylnaphthane,2,2,5,5-tetramethyl-3-hexanone,cyclooctanone,cyclododecanone with respectively,were studied.

研究了离子液体三溴化1-丁基-3-甲基咪唑[Br3]对2-戊酮、4-甲基苯乙酮、4-甲氧基苯乙酮、6-甲氧基-2-乙酰基萘、2,2,5,5-4-甲基-3-己酮、环辛酮、环十二酮、丁醛等羰基化合物的α-溴化反应。

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 paper, the improvement of synthetic method of 2-acetylaminotropone is introduced. 3-Acetyltropolone reacted with low concen-tration methylamine solution and solvent was directly evaporated in reduce pres-sure to give 2-acetyl-7 -methylaminotropone in good yield. The compound reacted with phenyltrimethylammonium tribromide to give two new compounds.

本文介绍2-乙酰基-7-甲胺基酮合成方法的改进——用挥发性小的低浓度甲胺溶液与3-乙酰基酚酮反应;和采用直接减压蒸除溶剂法分离产品,得到较好产率的2-乙酰基-7-甲胺基酮;用化合物与三溴化苯基三甲铵反应,得到两种至今未见文献报道的新化合物。

Treatment of pterin (2-amino-4-hydroxy-pteridine) derivatives with N,N-dimethylformamide dimethylacetal [1,(CH 3) 2NCH(OCH 3) 2] usually gave corresponding N 2-(N,N-dimethylaminomethylene)- pterin derivatives in polar solvents.

用N ,N 二甲基甲酰胺缩二甲醇 [(CH3 ) 2 NCH(OCH3 ) 2 ,1]和蝶呤(2 氨基 4 羟基蝶啶)衍生物在极性有机溶剂中反应一般得到脒化产物:N2 (N ,N 二甲基氨基亚甲基)-蝶呤衍生物。

Moreover, the protein-free spreading-free spreading technique, involvingbenzyldimethyl-alkyammonium bromide and the denaturing agent formamide, wasestablished. With very low DNA concentration, the fully extended DNA samples for linearDNA can be prepared.

采用Sephadex色谱柱分离,保温稀释的DNA溶液,不仅可除去DNA链上吸附的盐,而且可使盘绕一起的DNA链部分展开;在此基础上,通过采用苯二甲基辛基溴化胺-甲酰胺微量展层技术,可使纳克级DNA完全展开到云母基底上。

Optimum conditions are as follows: DMF is used as solvent, compound quaternary ammonium salt as catalyst, n(p-nitrochloro benzene):n=1: 1.2, m:m(p-nitrochloro benzene)=4%, m:m(p-nitrochloro benzene)1:1, and reacted under 155~160℃ for 18 h; reduction reaction is carried out in methanol with Raney nickel, which is used as catalyst; the raw product is added an antioxidant, and distilled simply under reduced pressure to obtain 4-fluoroaniline with excellence quality, purity is over 99.5%, total yield is 89.3%.

实验结果表明,氟化反应的最佳条件为:二甲基甲酰胺为溶剂、复合季铵盐为催化剂,n:n=1:1.2,m(催化剂:m=4%,m:m=1:1,于155~160℃下反应18h;还原反应在甲醇中进行,以阮内镍为催化剂;粗产品加入抗氧剂,减压条件下简单蒸馏得高品位的对氟苯胺。

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此刻阴唇已经几乎完全的缝在一起了,排除多余淤血体液的管子和Foley导管从顶端冒出来。

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