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溴乙酸甲酯置于四丁基氯化铵体系中,用 乙腈 作为反应溶剂,化学反应生成 氯乙酸甲酯
参考文献:Atrp中卤素交换的机理
标题:Atrp中卤素交换的机理
摘要:详述的机制研究揭示atrp该卤素交换(he),可能会发生不仅通过自由基途径(原子转移),而且还通过离子通道(s ñ 2反应),因为铜(i)(l)x和cu (II)(l)x 2络合物包含弱缔合的卤化物阴离子,其可参与与烷基卤化物(atrp引发剂)的s N 2反应.两种途径都进行了动力学研究,并定量评估了七个烷基卤化物和三个cu (i)(l)cl配合物对he过程的贡献.自由基途径主导着3°和2°烷基溴与高活性配合物(例如cu (i))的he过程(tpma)cl.有趣的是,离子途径在1°烷基溴和活性较低的atrp催化剂中占主导地位.这些研究还表明,烷基卤化物阴离子的缔合度取决于铜络合物的结构.另外,自由基途径伴随着反向反应,例如自由基被钝化为烷基溴,以及烷基氯的活化,从而降低了卤素交换的效率.
DOI:10.1021/ma201035U

专利信息

专利号:US-4288608-A
优先权日:1978-06-01
标题:Synthesis of anthracyclines
发明人：JOHNSON FRANCIS; KIM KYOUNG S
权利人:RESEARCH CORP
摘要:There is provided a novel method of synthesizing certain heterocyclic quinones. In particular there is provided a novel and regiospecific synthesis of 9-acetyl-6,11-dihydroxy-4-methoxy-7,8,9,10-tetrahydronaphthacene-5,12-quinone (7,9-dideoxydaunomycinone) which is known intermediate in the synthesis of daunomycinone. There is also provided a method of preparing analogs of 7,9-dideoxydaunomycinone which thus provide for the preparation of known and desired analogs of daunomycinone. Daunomycinone is a known compound which is an intermediate in the preparation of the clinically accepted naturally-occurring antitumor antibiotics daunomycin and its derivitive adriamycin.

专利号:WO-2004037772-A1
优先权日:2002-10-22
标 题 :Convenient and scalable synthesis of ethyl n-[(2-boc-amino) ethyl] glycinate and its hydrochloride salt
发明人：HUDSON ROBERT H E; VIIRRE RUSSELL D
权利人:UNIV WESTERN ONTARIO; HUDSON ROBERT H E; VIIRRE RUSSELL D
摘要:The present invention discloses an improved synthesis of ethyl N-[(2-Boc-amino)ethyl]glycinate and its hydrochloride salt. The synthesis is based on the reductive alkylation of Boc-ethylenediamine with ethyl glyoxylate hydrate and furnishes the title compound in near quantitative yield and high purity without chromatography. This compound is suitable, as is, for the synthesis peptide nucleic acid monomers. Further, conversion to the hydrochloride salt provides a stable, non-hygroscopic solid that is a convenient form for handling and storage.

专利号:US-5057624-A
优先权日:1989-03-31
标 题 :Process for the synthesis of the n-methyl-3,4-dimethoxyphenylethylamine
发明人：CANNATA VINCENZO; TAMERLANI GIANCARLO; ZAGNONI GRAZIANO
权利人:ALFA WASSERMANN SPA
摘要:New process for the synthesis of the N-methyl-3,4-dimetoxyphenylethylamine of formula ##STR1## intermediate in the synthesis of the drug internationally known as verapamil. The process starts from the 3,4-dimethoxybenzaldehyde which, by means of a Darzens condensation, gives an epoxyester that, by alkaline hydrolysis and subsequent decarboxylation, gives the 3,4-dimethoxyphenylacetaldehyde. This aldehyde gives the amine of formula I by reaction with monomethylamine followed by reduction with sodium borohydride.

专利号:US-5097058-A
优先权日:1987-04-08
标题:Process for the synthesis of the α-(-methyl-ethyl)-3,4-dimethoxybenzene-acetonitrile
发明人：CANNATA VINCENZO; TAMERLANI GIANCARLO; ZAGNONI GRAZIANO
权利人:ALFA WASSERMANN SPA
摘要:New process for the synthesis of the α-(1-m.ethylethyl)-3,4-dimethoxyacetonitrile of formula (I): ##STR1## which is known as an intermediate in the synthesis of the drug internationally known as verapamil. The process starts from the isobutyryl-3,4-dimethoxybenzene of formula (II): ##STR2## which, by means of the Darzens condensation, gives an epoxyester which, by alkaline hydrolysis and subsequent decarboxylation, gives the α-(1-methylethyl)-3,4-dimethoxybenzeneacetaldehyde. This product is reacted with hydroxylamine to obtain the corresponding oxime that, by dehydration, gives the nitrile of formula I.

专利号:US-10280189-B2
优先权日:2012-07-17
标题:Method for the synthesis of aminoalkylenephosphonic acid
发明人：BURCK SEBASTIAN; LECLERCQ CEDRIC NICOLAS; NOTTE PATRICK
权利人:MONSANTO TECHNOLOGY LLC
摘要:A method for the synthesis of an aminoalkylenephosphonic acid or its phosphonate esters including the following steps: a) forming, in the presence of an aldehyde or ketone and an acid catalyst, a reaction mixture by mixing a compound having at least one HNR 1 R 2 moiety or a salt thereof, with a compound having one or more P—O—P anhydride moieties, the moieties having one P atom at the oxidation state (+III) and one P atom at the oxidation state (+III) or (+V), wherein the ratio of moles of aldehyde or ketone to N—H moieties is 1 or more and wherein the ratio of N—H moieties to P—O—P anhydride moieties is 0.3 or more, and b) recovering the resulting aminoalkylenephosphonic acid having compound or its phosphonate esters.

专利号:US-3681428-A
优先权日:1968-10-24
标 题:Synthesis of phosphorane compounds
发明人：ROBERTS DONALD LEROY; RICE WILLIAM YATES JR
权利人:REYNOLDS TOBACCO CO R
摘要:Synthesis of phosphorane compounds by reaction of a triarylphosphine, an Alpha -haloester and an amine.