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The resultant was hydrogenised to remove protective group of amino group, then the product was reacted with NaNO2 to give diazonium salt, which was conjugated with salicylic acid, hydroxybenzene, N-salicyloyl glycine acid to get azo derivatives of 4-ASA.

本文首先对4-ASA的氨基和羟基进行了选择性保护,通过氢化还原法选择性脱除氨基的保护基,然后将氢化产物制成重氮盐,通过与水杨酸、苯酚和水杨酰甘氨酸发生反应生成4-ASA的偶氮衍生物,最后在碱性条件下水解得到最终产物。

Methods 4-Hydroxybenzonitrile (2) as the starting material was transformed to 4-hydroxy-thiobenzamide (3) via thioformylation. And ethyl 2-(4-hydroxyphenyl)-4-methylthiazole-5-carboxylate (4), which was synthesized via cyclization from 3, was treated with hexamethylenetetramine to generate the intermediate ethyl 2-(3-formyl-4-hydroxyphenyl)-4-methylthiazole-5-carboxylate (5). The target compound febuxostat (1) was obtained from 5 by etherification, cyanidation, hydrolysis.

以羟基苯腈为原料,经硫代甲酰化得到对羟基硫代苯甲酰胺(3),3经环合得到2-(4-羟基苯基)-4-甲基-噻唑-5-羧酸乙酯(4),4与乌洛托品反应,得到中间体2-(3-甲酰基-4-羟基苯基)-4-甲基-噻唑-5-羧酸乙酯(5),之后再经醚化、氰化、水解得到目标产物(1)。

The titled compound as an intermediate for preparing muscone is obtained by reacting a tetradecanedioic acid as the starting material with a chlorinating agent——chlorosulfoxide,followed by reacting the resultant reaction product on halogenomethylzinc .

采用直链十四碳二元酸为起始原料,先以氯化亚砜进行酰化,所得酰氯直接与甲基锌试剂反应进行甲基化,从而制得了合成麝香酮的重要中间体2,15-十六烷二酮,产物结构经1HNMRI、R确认。

In the study of peptide formation from phosphoryl aspartic acid with ethyl alanine, the N-phosphoryl peptide ester was isolated and identified by 1D and 2D NMR. It was found that only α-dipeptide ester, no β-dipeptide ester, was formed in the reaction.

实验发现N-磷酰化极性氨基酸在没有活化剂、缩合剂的水溶液中能够发生成肽反应,且生成的磷酰化二肽具有方向性:成肽产物的N端氨基酸来自N-磷酰化氨基酸,成肽反应发生在其C端。

Ethoxycarbonyl-4,5-dimethyl-pyrrole (7) was prepared from ethylacetoacetate, ethyl formate and methyl ethyl ketone via oximination, Claisen condensation, and reductive condensation. The bromization of compound 7 gave 2-ethoxycarbonyl-3-bromo-4,5-dimethyl-pyrrole(8), which could be transferred to 2-ethoxy-carbonyl-3-brome-4-methyl-5-formyl-pyrrole (9) by the formolation.

由乙酰乙酸乙酯、甲酸乙酯及丁酮等原料经过肟化、Claisen缩合、还原缩合成环得到2-乙氧羰基-4,5-二甲基-吡咯(7),溴化生成2-乙氧羰基-3-溴4,5-二甲基-吡咯(8),最后经过甲酰化反应得到目标产物2-乙氧羰基-3-溴-4-甲基-5-甲酰基-吡咯(9)。

ABSTRACT This thesis focused on the studies of setereoselectively total synthesis of naturally occurring bisabolane sesquiterpenes and hydroxamic acid derivatives; it contains the following five parts: Part Ⅰ: Hydroformylation reaction have been taken an overview for past 40 years.

本论文主要对防风根烯类倍半萜天然产物和羟肟酸类化合物的全合成进行了研究,内容概要如下:一、对近年来氢甲酰化反应——特别是不对称氢甲酰化反应作了详尽的综述。

Methods: 2ethyl aniline was used as starting material of the synthesis and was processed by acetic anhydride acylation, strong nitric acid nitraction at low temperature, and desacyl synthesis to produce 2ethyl5nitro aniline. The product was then synthesized to 3methyl6nitro1Hindazole by using ringclosing reaction in the presence of NaNO2, and then ethylated to obtain 2,3diethyl6 nitro2Hindazole. The latter compound was then reduced by SnCl2/Hcl to get target compound 2,3diethyl6nitro2Hindazole.

以2乙基苯胺为原料经醋酐酰化、浓硝酸低温硝化及去酰基保护合成2乙基5硝基苯胺,后用亚硝酸钠关环得3甲基6硝基1H吲唑,经硫酸二甲酯甲基化得2,3二甲基6硝基2H吲唑,最后用氯化亚锡将其还原得到目标产物,通过1H NMR确定结构与目标产物一致。

Methods: 2-ethyl aniline was used as starting material of the synthesis and was processed by acetic anhydride acylation, strong nitric acid nitraction at low temperature, and desacyl synthesis to produce 2-ethyl-5-nitro aniline. The product was then synthesized to 3-methyl-6-nitro-lH-indazole by using ring-closing reaction in the presence of NaNO2, and then ethylated to obtain 2, 3-diethyl-6- nitro-2H-indazole. The latter compound was then reduced by SnC12/Hcl to get target compound 2, 3-diethyl-6-nitro-2H-indazole.

以2-乙基苯胺为原料经醋酐酰化、浓硝酸低温硝化及去酰基保护合成2-乙基-5-硝基苯胺,后用亚硝酸钠关环得3-甲基-6-硝基-1H-吲唑,经硫酸二甲酯甲基化得2,3-二甲基-6-硝基-2H-吲唑,最后用氯化亚锡将其还原得到目标产物,通过1HNMR确定结构与目标产物一致。

Piperidinecarboxylic acid is used as the raw material and acetic acid as the acylating agent, followed by the addition of some acetic anhydride in the later stage to get an important organic intermediate n-acetylpiperidine-4 carboxylic acid in the yield of 92%. Toluene is used as the solvent instead of sulfinyl chloride in the acyl chlorination to produce n-acetylpiperidine-4-carbonyl chloride with the yield of 97%.

以4-哌啶甲酸为原料、醋酸为酰化剂,后期加入少量醋酸酐反应得到中间体N-乙酰基哌啶-4-甲酸,收率92%;在甲苯溶剂中进行酰氯化得目标产物N-乙酰基哌啶-4-甲酰氯,收率97%。

The experiment takes carbolic acid as raw material , adopt acetophenetidin-rization, Fries weight row , the oxime have molten , Beckmann weight row combining method has got target outcome to acetophenetidin aminophenol, total recovery is under using acetone as catalysator in the best reaction temperature and the best reaction time: 40.5%.

在线等翻译~请哪位好心人帮我翻译一下我的毕业论文摘要~谢谢了。不要网站或者软件直译的!摘要本实验以苯酚为原料,采用乙酰化、Fries重排、肟化、Beckmann重排的合成方法得到了目标产物对乙酰氨基酚,用丙酮作催化剂在最佳反应温度和最佳反应时间下总收率为:40.5%。

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