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甲酰化

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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)。

Besides,through Arbuzov reaction,Vilsmer-Haack Hydroformylation,Wittig-Horner reaction,nitryl hydrogenation deoxidize,and imidization five steps synthesized another compound which included hole-transporting,electron-transporting and luminescence materials.

此外,又通过Arbuzov反应、Vilsmer-Haack甲酰化反应、Wittig-Horner反应生成二苯乙烯、硝基加氢还原、酰亚胺化5步反应合成了一种集空穴传输-电子传输-发射三位一体的新型苝酰亚胺化合物。

HCo 〓-catalyzed hydroformylation and isomerization of allene and propyne Allene hydroformylation favors the linear anti-Markovnikov product in high regioselectivity both kinetically and thermodynamically. The origin of this regioselectivity comes from the enhanced stability of the η〓-allylic intermediate (η〓-CH〓CHCH〓 Co 〓.

HCo〓催化的丙二烯和丙炔氢甲酰化反应及异构化反应 HCo〓催化丙二烯氢甲酰化反应的区域选择性主要由不可逆的丙二烯插入步骤决定,动力学和热力学因素都有利于形成anti-Markovnikov中间物种(η〓-CH〓CHCH〓)Co〓,形成Markovnikov中间物种Co〓是不具有竞争性的。

In the fifth chapter, a series of betulin derivatives including 28-acetoxybetulin, 28-tritylbetulin, 28-benzoylbetulin, 3-0-P-D-glucopyranoside of betulin and some betulinic acid conjugate containing amino acid were synthesized and confirmed by MS and NMR.

第五章分别合成得到了乙酰化白桦酯醇、28-苯甲酰化白桦酯醇、28-三苯甲基化白桦酯醇、3-O-β-D-glucopyranoside of betulin和一系列的白桦酯酸苷氨酸的衍生物,并分别对其进行了结构鉴定。

The effects of solvent on the bromization reaction and oxidant on the formolation reaction of the target product were studied. The results show that the optimum solvent for the bromization reaction and the optimum oxidant for the formolation reaction of the target product were carbon tetrachloride and ceric ammonium nitrate, and their yields were 86.7% and 89.3% respectively.

同时就溴化反应中的溶剂以及甲酰化反应中的氧化剂对两类反应的影响分别进行了研究,结果表明溴化反应的最佳溶剂为四氯化碳,反应产率达到86.7%,甲酰化反应的最佳氧化剂为硝酸铈铵,产率达到89.3%。

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)。

The key intermediate 3-methylaminopiperidine was synthesized from 3-methylaminopyridine by two methods,formylation and lithium aluminium hydride reduction or condensation with triethyl orthoformate and sodium borohydride reduction,and then hydr...

以3-氨基吡啶为原料,分别通过甲酰化反应、氢化铝锂还原和原甲酸三乙酯缩合、硼氢化钠还原两种方法得到3-甲胺基吡啶,最后经催化氢化得到中间体3-甲胺基哌啶。

The key intermediate 3- methylaminopiperidine was synthesized from 3-methylaminopyridine by two methods, formylation and lithium aluminium hydride reduction or condensation with triethyl orthoformate and sodium borohydride reduction, and then hydrolysis.

以3-氨基吡啶为原料,分别通过甲酰化反应、氢化铝锂还原和原甲酸三乙酯缩合、硼氢化钠还原两种方法得到3-甲胺基吡啶,最后经催化氢化得到中间体3-甲胺基哌啶。

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。

However, the rhodium process with oil compounds encounter problems due to the thermal sensitivity of the high boiling point oxo-products, which cannot be isolated from the homogeneous reaction mixture by distillation.

采用~1H-NMR和FT-IR谱分析了油醇的氢甲酰化反应产物,证实了其结构为甲酰基十八碳醇,且甲酰基的位置可以在主碳链的中间或端位。

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