4-苯丁酸甲酯置于lithium Aluminium Tetrahydride,三溴化磷体系中,化学反应生成4-苯基-1-丁基溴 参考文献:Photolysis Of 2-Phenylethyl And 4-Phenyl-1-Butyl Halides In Alcoholic Solvents 标题:Photolysis Of 2-Phenylethyl And 4-Phenyl-1-Butyl Halides In Alcoholic Solvents 摘要: Doi:10.1016/s0040-4020(01)87368-3
专利号:WO-2016037298-A1 优先权日:2014-09-11 标题 :Method for the enantioselective synthesis of 2(s)-amino-6-boronohexanoic acid (abh) and purification thereof 发明人:PREITE MARCELO DANIEL; MANRIQUEZ MUJICA JUAN MANUEL; CORREA VARGAS JORDAN MAURICIO; ITURRIAGA AGUERA RODRIGO MANUEL; CASANELLO TOLEDO PAOLA CECILIA; KRAUSE LEYTON BERNARDO JAVIER 权利人:UNIV PONTIFICIA CATOLICA CHILE 摘要:The invention relates to a method for the enantioselective synthesis and purification of 2(S)-amino-6-boronohexanoic acid (ABH) and the preparation of the corresponding synthetic intermediates. The method comprises the preparation of ABH from BPB-Ni-Gly, which is treated with a strong base in a suitable solvent, and is made to react with 2-(4-lower bromoalkyl)benzo[d] [1,3,2]dioxaborol, where the lower alkyl is an alkyl with between 1 and 6 carbon atoms, preferably 2-(4- bromo-butyl)benzo[d][1,3,2]dioxaborol, while stirring, in a nitrogen atmosphere and with a cryogenic bath at a low temperature (-50°C), in order to then permit same to reach ambient temperature, removing the cryogenic bath, before neutralising in aqueous medium with a weak organic acid, and extracting with dichloromethane, drying the resulting organic extract which is subsequently filtered and vacuum evaporated. The resulting alkylated complex is dissolved in a C1-C5 alcohol, adding a hydrochloric acid, refluxing in a nitrogen atmosphere, and is subsequently cooled to ambient temperature, and concentrated in order to achieve the precipitation of (S)-2-[N-(N'- benzylprolyl) amino]benzophenone (BPB), as the hydrochloride salt, filtering and extracting with dichloromethane, and after dissolving the aqueous phase of the filtrate in water, it is treated with ammonia concentrated to pH 9, and once again extracted with dichloromethane, the ammoniacal aqueous phase being vacuum evaporated until dry, in order to produce crude ABH, as the ammonium salt, which is subsequently purified by means of ion-exchange chromatography. The invention also relates to a method for preparing the Gly-Ni-BPB complex, 2-(4- bromo-butyl)benzo[d][1,3,2]dioxaborol, which is used as an alkylating agent in the form of a borate side chain, and (S)-N- benzylproline (BP).
专利号:US-2024025925-A1 优先权日:2022-07-20 标题 :Systems and methods for preparation of highly reactive alkali metal dendrites for the synthesis of organolithium reagents 发明人:THOMAS ANDY A; CROCKETT MICHAEL P; AGUIRRE LUPITA S; JIMENEZ LEONEL B; HSU HAN-HSIANG 权利人:TEXAS A & M UNIV SYS 摘要:Systems and methods for formation of highly reactive alkali dendrites are provided. For example, in some embodiments alkali metals are dissolved in ammonia to form metal electrides after which the ammonia is removed via vacuum to reveal highly activated metal surfaces in the form of crystalline alkali dendrites. The alkali dendrites can mimic powders but have the advantage of being freshly prepared from inexpensive and readily available metal sources. These uniquely activated metals exhibit enhanced reactivity comparatively to similar off the shelf sources of the corresponding metals. For example, the dendrites can have about 100 times greater surface area than conventional metal sources and/or be about 19 times more reactive than powders that serve as the industry standard for the preparation of organometallic compounds. After surface activation, these metals can be used to prepare various organometallic reagents.
专利号:US-4710513-A 优先权日:1979-08-17 标 题:Substituted pyranone inhibitors of cholesterol synthesis 发明人:WILLARD ALVIN K; NOVELLO FREDERICK C; HOFFMAN WILLIAM F; CRAGOE JR EDWARD J 权利人:MERCK & CO INC 摘要:6-Phenyl-, phenylalkyl- and phenylethenyl-4-hydroxytetrahydropyran-2-ones in the 4(R)-trans stereoisomeric forms are potent inhibitors of cholesterol synthesis by virtue of their ability to inhibit the enzyme, 3-hydroxy-3-methylglutaryl-coenzyme A reductase.
专利号:US-4459422-A 优先权日:1979-08-17 标 题:Substituted pyranone inhibitors of cholesterol synthesis 发明人:WILLARD ALVIN K; NOVELLO FREDERICK C; HOFFMAN WILLIAM F; CRAGOE JR EDWARD J 权利人:MERCK & CO INC 摘要:6-Phenyl-, phenylalkyl- and phenylethenyl-4-hydroxytetrahydropyran-2-ones in the 4(R)-trans stereoisomeric forms are potent inhibitors of cholesterol synthesis by virtue of their ability to inhibit the enzyme, 3-hydroxy-3-methylglutaryl-coenzyme A reductase.
专利号:US-4375475-A 优先权日:1979-08-17 标 题 :Substituted pyranone inhibitors of cholesterol synthesis 发明人:WILLARD ALVIN K; NOVELLO FREDERICK C; HOFFMAN WILLIAM F; CRAGOE JR EDWARD J 权利人:MERCK & CO INC 摘要:6-Phenyl-, phenylalkyl- and phenylethenyl-4-hydroxytetrahydropyran-2-ones in the 4(R)-trans stereoisomeric forms are potent inhibitors of cholesterol synthesis by virtue of their ability to inhibit the enzyme, 3-hydroxy-3-methylglutaryl-coenzyme A reductase.
专利号:US-4567289-A 优先权日:1979-08-17 标 题 :Substituted pyranone inhibitors of cholesterol synthesis 发明人:WILLARD ALVIN K; NOVELLO FREDERICK C; HOFFMAN WILLIAM F; CRAGOE JR EDWARD J 权利人:MERCK & CO INC 摘要:The methyl, ethyl, n-propy, 2-(acetylamino)ethyl, or 1-(2,3-dihydroxy)propyl ester of E-(3R,5S)-7-(4'-fluoro-3,3',5-trimethyl[1,1'-biphenyl]-2-yl)-3,5-dihyd roxy-6-heptenoic acid of structural formula: are HMG-CoA reductase inhibitors useful in the treatment of conditions associated with hypercholesterolemia.