专利号:US-5455367-A 优先权日:1993-04-22 标 题:Method for the synthesis of silanes or organosilicon hydrides by the reduction of the corresponding silicon halides or organosilicon halides 发明人:KLEIN KLAUS-DIETER; KNOTT WILFRIED; KOERNER GOETZ 权利人:GOLDSCHMIDT AG TH 摘要:A method for the synthesis of silanes or organosilicon hydrides by the reduction of the corresponding silicon halides or organosilicon halides with a magnesium hydride in a liquid reaction medium is carried out by utilizing the following distinguishing features: n a) the use of non-pyrophoric, preferably autocatalytically produced, storage magnesium hydride as magnesium hydride, n b) the use of conventional ethers as reaction medium, and n c) the continuous removal of the magnesium halide formed being deposited on the surface of the magnesium hydride particles during the reaction by the action of mechanical energy or ultrasound so as to form a fresh surface.
专利号:US-7189864-B2 优先权日:1990-11-19 标 题:Method of preparing intermediates useful in synthesis of retroviral protease inhibitors 发明人:NG JOHN S; PRZYBYLA CLAIRE A; MUELLER RICHARD A; VAZQUEZ MICHAEL L; GETMAN DANIEL P 权利人:SEARLE & CO 摘要:A synthesis is described for intermediates which are readily amenable to the large scale preparation of hydroxyethylurea-based chiral HIV protease inhibitors. The method includes forming a diastereoselective epoxide from a chiral alpha amino aldehyde.
专利号:US-6022996-A 优先权日:1990-11-19 标 题 :Method for making intermediates useful in synthesis of retroviral protease inhibitors 发明人:NG JOHN S; PRZYBYLA CLAIRE A; MUELLER RICHARD A; VAZQUEZ MICHAEL L; GETMAN DANIEL P 权利人:SEARLE & CO 摘要:A synthesis is described for intermediates which are readily amenable to the large scale preparation of hydroxyethylurea-based chiral HIV protease inhibitors. The method includes forming a diastereoselective epoxide from a chiral alpha amino aldehyde.
专利号:EP-0641333-B1 优先权日:1992-05-20 标 题 :Method for making intermediates useful in synthesis of retroviral protease inhibitors 发明人:NG JOHN S; PRZYBYLA CLAIRE A; MUELLER RICHARD A; VAZQUEZ MICHAEL L; GETMAN DANIEL P 权利人:SEARLE & CO; MONSANTO CO 摘要:A synthesis is described for intermediates which are readily amenable to the large scale preparation of hydroxyethylurea-based chiral HIV protease inhibitors. The method includes forming a diastereoselective epoxide compound of formula (I) from a chiral alpha amino aldehyde and halomethyllithium as an organometallic methylene-adding reagent. In formula (I) R<1> is selected from alkyl, aryl, cycloalkyl, cycloalkylalkyl and arylalkyl, which are optionally substituted with a group selected from alkyl, halogen, NO2, OR<9> or SR<9>, where R<9> represents hydrogen or alkyl; and P<1> and P<2> independently are selected from amine protecting groups, including but not limited to, arylalkyl, substituted arylalkyl, cycloalkenylalkyl and substituted cycloalkenylalkyl, allyl, substituted allyl, acyl, alkoxycarbonyl, aralkoxycarbonyl and silyl.
专利号:EP-0855388-B1 优先权日:1993-11-23 标 题 :Method for making intermediates useful in synthesis of retroviral protease inhibitors 发明人:NG JOHN S; PRZYBYLA CLAIRE A; MUELLER RICHARD A; VAZQUEZ MICHAEL L; GETMAN DANIEL P; FRESKOS JOHN J; DECRESCENZO GARY A; BERTENSHAW DEBORAH E; HEINTZ ROBERT M; ZHANG SUHONG; LIU CHIN; LANEMAN SCOTT A 权利人:SEARLE & CO 摘要:A synthesis is described for intermediates which are readily amenable to the large scale preparation of hydroxyethylurea-based chiral HIV protease inhibitors. The method includes forming a cyanohydrin from a chiral alpha amino aldehyde.
专利号:WO-03068806-A1 优先权日:2002-02-14 标 题 :Solid phase peptide synthesis on silica 发明人:GROARKE MICHELLE 权利人:JOHNSON MATTHEY PLC; GROARKE MICHELLE 摘要:A method for peptide synthesis is described, comprising steps of forming an organofunctional silica by reaction of an alkyl silicate, an organofunctional silane and water, optionally in the presence of a template compound; removing the template compound if present; reacting said organofunctional silica with a first protected amino acid to produce a tethered protected amino acid; deprotecting the tethered protected amino acid; reacting at least one further protected amino acid with said tethered deprotected amino acid to form a tethered peptide, and removing the peptide from the organofunctional silica. Preferably, prior to reaction of the first protected amino acid, the organofunctional silica is reacted with at least one linking compound to form a linker-modified organofunctional silica with which the first protected amino acid is reacted. A method for preparing an organfunctional silica by the co-hydrolysis of an alkyl silicate and an organofunctional silane is depicted below. The wavy line represents the silicon atom on or within the resulting silica material formula (I). A reaction of a protected amino acid with an organofunctional silica to provide a tethered protected amino acid is depicted below formula (II).
参考文献:10.1007/s41061-019-0245-4 摘要:Peng W, Vessally E, Arshadi S, Monfared A, Hosseinian A, Edjlali L. Cross-Dehydrogenative Coupling Reactions Between C(sp)-H and X-H (X = N, P, S, Si, Sn) Bonds: An Environmentally Benign Access to Heteroatom-Substituted Alkynes. Top Curr Chem (Cham). 2019 Jul 04;377(4):20. doi: 10.1007/s41061-019-0245-4.