乙酰化氧

Methods Starting from 2-chloro-4-nitrophenol and 2- pyridine hydrochlorid, 3-chloro-4-(pyridin-2-ylmethoxy) aniline was obtained via etherization and reduction. The obtained aniline coupled with N-(4-chloro-3-cyano-7-ethoxyquinolin-6-yl) acetamide to give 4-[3-chloro-4-(2-pyridylmethoxy) phenylamino]-3-cyano-7-ethoxy-6-N-acetylaminoquinoline. And then it was deacetylated, followed by reacting with4- but-2-enoyl chloride to yield the target compound neratinib.

以2-氯－4-硝基苯酚和2-氯甲基吡啶为起始原料，经醚化、硝基还原得到3-氯－4-（吡啶－2-甲氧基）苯胺，3-氯－4-（吡啶－2-甲氧基）苯胺与3-氰基－6-乙酰氨基－7-乙氧基－4-氯喹啉反应得到3-氰基－6-乙酰氨基－4-［3-氯－4-（吡啶－2-甲氧基）苯氨基］－7-乙氧基喹啉，3-氰基－6-乙酰氨基－4-［3-氯－4-（吡啶－2-甲氧基）苯氨基］－7-乙氧基喹啉去乙酰保护基后，与-4-二甲氨基－2-丁烯酰氯经酰化反应得到ner-atinib。

A selective and mild PS-DIB/ionic-liquid immobilized 2, 2, 6, 6-tetramethyl-piperidin-4-ol-N-oxyl catalytic oxidation procedure of alcohols to the corresponding aldehydes and ketones in ionic liquid BF4 at room temperature was developed. The oxidant PS-DIB was prepared via the iodation and acetylation of polystyrene resin. For the preparation of the ionic-liquid immobilized TeMPO catalyst, 4-(2, 2, 6, 6-Tetramethyl-1-oxyl-4-piperidoxyl)butyl bromide was first synthesized from TeMPO and 1, 4-dibromobutane.

将聚苯乙烯树脂先碘化再乙酰基化，制得了负载型二乙酰氧碘苯作为氧化剂。2， 2， 6， 6-四甲基－N-氧自由基哌啶醇与1， 4-二溴丁烷反应生成4-溴丁氧基－2， 2， 6， 6-四甲基－哌啶－1-氧化物，再与N-甲基咪唑发生季铵化反应，生成的溴化季铵盐与四氟硼酸钠进行离子交换制得氟硼酸型2， 2， 6， 6-四甲基－N-氧自由基哌啶负载离子液体。

A selective and mild PS-DIB/ionic-liquid immobilized TEMPO catalytic oxidation procedure of alcohols to the corresponding aldehydes and ketones in ionic liquid BF4 at room temperature was developed. The oxidant PS-DIB was prepared via Iodation and acetylation of polystyrene resin. For the preparation of the ionic-liquid immobilized TEMPO catalyst, 4-(2,2,6,6-Tetramethyl-1-oxyl-4-piperidoxyl)butyl bromide was first synthesized from 2,2,6,6-tetramethyl-piperidin-4-ol-N-oxyl and 1,4-dibromobutane.

将聚苯乙烯树脂先碘化再乙酰基化，制得了负载型二乙酰氧碘苯(diacetoxyiodo polystyrene，PS-DIB)作为氧化剂。2，2，6，6-四甲基-N-氧自由基哌啶醇(2，2，6，6-tetramethyl-piperidin-4-ol-N-oxyl，TEMPO)与1，4-二溴丁烷反应生成4-溴丁氧基-2，2，6，6-四甲基-哌啶-1-氧化物，再与N-甲基咪唑发生季铵化反应，生成的溴化季铵盐与四氟硼酸钠进行离子交换制得氟硼酸型2，2，6，6-四甲基-N-氧自由基哌啶负载离子液体TEMPO-IL。

The synthesis of nalbuphine hydrochloride from thebaine as starting material was through following processes:oxidation,high-pressure hydrogenation,acetylation,removing methyl of 3-methoxy,hydrolysis,condensation,reduction and finial salification.

以蒂巴因为起始原料，经氧化、高压氢化、乙酰化、氰化、脱3-位甲氧基的甲基、水解、缩合、还原、成盐，合成了盐酸纳布啡，总收率达18。

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)。

Ib was synthesized by condensation of phthalic anhydride with 2-methylresorcinol in fused AlCl〓/NaCl (5∶1), followed by selective acetylation, methylation, NBS bromination and condensation with sodium ethoxide.

邻苯二甲酸酐在熔融的三氯化铝-氯化钠(5：1)中和-2，6-二羟基甲苯环合得1，3-二羟基-2-甲基蒽醌〓后经选择性乙酰化、甲基化、NBS溴化、乙醇钠缩合得1-甲氧基-2-乙氧甲基-3-羟基蒽醌。

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。

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

Respectively, glutamic acid derivatized β-CD has been synthesized with epoxy chloropropane as the intermediate, a water-insoluble yellow liquid was got after the acetylating of the by using acetic anhydride, which was used as a novel gas chromatographic CSP; A water-soluble β-CD polymer cross-linked with epoxy chloropropane has been synthesized, and the derivatives of β-CD polymer were synthesized by its alkylating and acetylating. The different β-CD derivatives were coated on silica capillary columns by dynamic method, the chromatographic properties and retention behaviors of the fused silica capillary columns were studied, the results showed that the β-CD derivatives had good stereoselectivity and separation results to some compounds, especially to various positional isomers and enantiomers.

本文还分别以环氧氯丙烷为中间体，合成了七{2，6-二-O-[3-(1，3-二羟基丙氨酸)]}-β-环糊精，再用醋酸酐将其乙酰化，得到了一种淡黄色粘稠液体，合成了一种新型的环糊精衍生物；以环氧氯丙烷作交联剂合成了一种水溶性的β-环糊精聚合物，再将其烷基化和酰基化，合成了β-环糊精聚合物的不同衍生物，用动态法将不同类型的β-环糊精衍生物涂渍在石英毛细管柱上，通过对所制备柱柱性能的测试和对一系列化合物的分离和保留行为的研究，结果表明所合成的β-环糊精衍生物对各类化合物，特别是对位置异构体和对映异构体具有较好的分离效果，显示了很强的立体选择性。

Bezaldehyde was used as protective agent in first method.S-Epichloeohydrin was aminated and acidulated to give(2S)-1-Amino-3-chloro-propanol Salts.The acetylation of (2S)-1-Amino-3-chloro-propanol by acetic anhydride produced the intermediate-N-[2--3-chloropropyl]acetamide.And then at 20℃,in the presence of lithium tert-butoxide,benzyl 3-fluoro-4-morpholinophenyl carbamate react with-N-[2--3-chloropropyl]acetamide to give linezolid in total yield of 43.6%.

路线一采用苯甲醛作保护剂，使S-环氧氯丙烷氨解、酸化生成S-1-氨基-3-氯-2-丙醇盐酸盐，然后经乙酰化反应后，生成中间体-N-[2-乙酰氧基-3-氯丙基]乙酰胺，再用N-(3-氟-4-吗啉苯基)氨基甲酸苄酯和中间体在催化剂叔丁醇锂存在下25℃反应生成利奈唑酮，总产率达到43.6%。

Do you know, i need you to come back

你知道吗，我需要你回来

Yang yinshu、Wang xiangsheng、Li decang,The first discovery of haemaphysalis conicinna.

1〕 杨银书，王祥生，李德昌。安徽省首次发现嗜群血蜱。