醋酸叔丁酯置于乙醚,氨,Sodium Amide体系中,化学反应生成 丙二酸单叔丁酯 参考文献:Hauser; Levine; Kibler,Journal Of The American Chemical Society,1946,Vol. 68,P. 27 标题:Hauser; Levine; Kibler,Journal Of The American Chemical Society,1946,Vol. 68,P. 27
专利号:US-4189583-A 优先权日:1978-04-26 标题 :Synthesis of 4A-aryl-decahydroisoquinolines 发明人:GLESS RICHARD D; RAPOPORT HENRY; WELLER DWIGHT D 权利人:U S OF AMERICA HEW SECRETARY 摘要:This invention relates to a process for the production of 4a-aryldecahydroisoquinolines where the aryl group is selected as 3-methoxy phenyl. These compounds are morphine analogs and show utility similar to the known morphine, codeine, and thebaine. In this process particular novelty is asserted for the production of a nipecotic ester ethyl 4-(3'-methoxyphenyl)-1-methyl piperidine-3-carboxylate. Furthermore, novelty is asserted for the step of conversion of the nipecotates through cyclization to cis- or trans-tert-butyl 1,6-dioxo-4a-(3'-methoxyphenyl)-2-methyldecahydroisoquinoline-7-carboxylate, which may also be easily converted to the keto amide, trans-1,6-dioxo-4a-(3'-methoxyphenyl)-2-methyldecahydroisoquinoline.
专利号:WO-2013057186-A1 优先权日:2011-10-19 标题 :Photolabile linker for the synthesis of hydroxamic acids 发明人:NIELSEN THOMAS E; QVORTRUP KATRINE 权利人:UNIV DANMARKS TEKNISKE 摘要:The present invention relates to a photolabile hydroxamate linker based on the o - nitroveratryl group and its application for multistep solid-phase synthesis and controlled photolytic release of hydroxamic acids. The invention provides a method for producing a solid support comprising a hydroxylamine - functionalized photolabile linker, and the so produced hydroxylamine - functionalized photolabile solid support. The invention further provides a method for synthesizing a one-bead-one compound library of hydroxamic acid derivatives on a photolabile linker, as well as a method for screening a library of hydroxamic acid derivatives.
专利号:WO-2007096751-A1 优先权日:2006-02-21 标题 :Process for the preparation of atorvastatin calcium 发明人:PATEL DHIMANT JASUBHAI; KUMAR RAJIV; DWIVEDI SHRI PRAKASH DHAR 权利人:CADILA HEALTHCARE LTD; PATEL DHIMANT JASUBHAI; KUMAR RAJIV; DWIVEDI SHRI PRAKASH DHAR 摘要:The present invention relates to process for the preparation of atorvastatin calcium. The process provides the novel approach for the synthesis of an important intermediate atorvastatin protected diol chemically (4R-cis)-6-[-2-[3-phenyl-4-(phenyl- carbamoyl)-2-(4-flourophenyl)-5-(1-methyl-ethyl)-pyrrol-1-yl]-ethyl]-2,2-dimethyl- [1,3]dioxane-4-yl-acetic acid-tertriay butyl ester for atorvastatin calcium i.e. [R- (R*,R*)]-2-(4-fluorophenyl-β,δ-dihydroxy-5-(1-methylethyl)-3-phenyl-4- [(phenylamino) carbonyl]-1H-pyrrole-1-heptanoic acid calcium salt (2:1). The present invention relates the use of amino side chain i.e [6-(2-aminoethyl)-2,2,-dimethyl- [1,3]dioxan-4-yl]-acetic acid tert-butyl ester and stetter compound i.e. 4-(4- FluoroÏ?henyl)-2-isobutryl-4-oxo-N-phenyl butryl amide as an important starting materials for the preparation of atorvastatin protected diol in the high yield and thereby the recovery of amino side chain with an industrially applicable process.
专利号:US-4283536-A 优先权日:1977-12-29 标 题:Preparation of vincadifformine and related derivatives 发明人:KUEHNE MARTIN E 权利人:UNIV VERMONT 摘要:This invention relates to the preparation of vincadifformine and related derivatives which are useful as starting material for the synthesis of among other alkaloids vincamine and other similar compounds possessing interesting psychopharmacologic properties. n A tetrahydro-β-carboline (II) is reacted with benzoyl chloride to provide a 2-benzoyl-1,2,3,4-tetrahydro-9H-pyrido-(3,4-b)-indole (III). Then compound (III) is reduced to give a 2-benzyl-1,2,3,4-tetrahydro-9H-pyrido-(3,4-b)-indole (IV). Thereafter, compound (IV) is transformed by t-butyl hypochlorite into a chloroindolenine derivative (V) which is immediately treated with a metal dialkylmalonate such as thallium t-butyl methyl malonate to give a dialkyl 3-benzyl-1,2,3,4,5,6-hexahydroazepino-(4,5-b)-indole-5,5-dicarboxylate (VI). Compound (VI) is then partly decarboxylated into a alkyl 3-benzyl-1,2,3,4,5,6-hexahydro-(4,5-b) indole-5-carboxylate (VII). Compound (VII) is hydrogenated to give an alkyl 1,2,3,4,5,6-hexahydroazepino-(4,5-b)-indole 5-carboxylate (VIII). In an alternative embodiment, compound (VI) can be hydrogenated to the corresponding dialkyl 1,2,3,4,5,6-hexahydroazepino-(4,5-b)-indole-5,5-dicarboxylate which is then decarboxylated into compound (VIII). Compound (VIII) is condensed with a functionalised aldehyde, typically a epoxy aldehyde or a haloaldehyde such as 1-bromo-4-formylhexane, to give vincadifformine or similar pentacyclic derivatives.
专利号:US-4435572-A 优先权日:1978-04-26 标题:Synthesis of ethyl-4(3'-methoxyphenyl)-1-methyl piperidine-3-carboxylate 发明人:RAPOPORT HENRY; WELLER DWIGHT D; CLESS RICHARD D 权利人:US HEALTH 摘要:This invention relates to a process for the production of 4a-aryldecahydroisoquinolines where the aryl group is selected as 3-methoxy phenyl. These compounds are morphine analogs and show utility similar to the known morphine, codeine, and thebaine. In this process particular novelty is asserted for the production of a nipecotic ester ethyl 4-(3'-methoxyphenyl)-1-methyl piperidine-3-carboxylate. Furthermore, novelty is asserted for the step of conversion of the nipecotates through cyclization to cis- or trans-tert-butyl 1,6-dioxo-4a-(3'-methoxyphenyl)-2-methyldecahydroisoquinoline-7-carboxylate, which may also be easily converted to the keto amide, trans-1,6-dioxo-4a-(3'-methoxyphenyl)-2-methyldecahydroisoquinoline.
专利号:US-7652168-B2 优先权日:2001-07-10 标 题 :Synthesis of taxol enhancers 发明人:CHEN SHOUJUN; SUN LIJUN; XIA ZHI-QIANG; KOVA KEIZO; ONO MITSUNORI 权利人:SYNTA PHARMACEUTICALS CORP 摘要:Disclosed is a method of preparing a thiohydrazide product compound from a hydrazide starting compound. The hydrazide starting compound is represented by Structural Formula (I): n nThe thiohydrazide product compound is represented by Structural Formula (II):n n nIn Structural Formulas (I)-(II), R 1 and R 2 are independently an aliphatic group, a substituted aliphatic group, an aryl group or a substituted aryl group, or R 1 and R 2 taken together with the carbon and nitrogen atoms to which they are bonded, form a non-aromatic heterocyclic ring optionally fused to an aromatic ring. When R 2 is an aryl group or a substituted aryl group, then R 5 is a hydrazine protecting group; and when R 2 is an aliphatic or substituted aliphatic group, then R 5 is —H or a hydrazine protecting group. R 10 is —H or a substituted or unsubstituted alkyl group. The method comprising the step of reacting the starting compound with a thionylating reagent.
[参考文献]: Jae Koo Lee, Et Al. Development Of An Enzyme-Linked Immunosorbent Assay For The Detection Of The Organophosphorus Insecticide Acephate. J Agric Food Chem. 2003 Jun 18;51(13):3695-703.
合成参考文献
摘要:Uyanik, M.; Ishihara, K., Science of Synthesis: Catalytic Oxidation in Organic Synthesis, (2017) 1, 661. 摘要:Lloyd, C. M.; Dowell, K. F.; Brittain, W. D. G., Science of Synthesis: Modern Strategies in Organofluorine Chemistry, (2025) 2.