D-吡喃木糖置于palladium On Activated Charcoal 吡啶,咪唑,Tris(Dibenzylideneacetone)Dipalladium(0) Chloroform Complex,氢氧化钾,Potassium Tert-Butylate,四丁基氟化铵,水,氢气,溴,二异丁基氢化铝,Potassium Carbonate,三乙胺,N,N-二异丙基乙胺,Zinc Dibromide体系中,用 四氢呋喃,乙醇,二氯甲烷,水,溶剂黄146,二甲基亚砜,乙酸乙酯,N,N-二甲基甲酰胺 作为反应溶剂,化学反应生成 阿法骨化醇 参考文献:A General Synthetic Route To A-Ring Hydroxylated Vitamin D Analogs From Pentoses 标题:A General Synthetic Route To A-Ring Hydroxylated Vitamin D Analogs From Pentoses 摘要:The Enzyne Needed For Coupling To A Cd-Ring Fragment,Namely,3S,5R-oct-1-En-7-Yne-3,5-Diol,In The Trost-Dumas Carbopalladation Route To 1 Alpha,25-Dihydroxyvitamin D-3 Was Synthesized From D-Xylose In 13 Steps And 21% Yield. DOI:10.1016/0040-4039(94)02209-T
专利号:US-2022267266-A1 优先权日:2019-07-09 标 题 :Improved, cost effective process for synthesis of vitamin d3 and its analogue calcifediol from ergosterol 发明人:DATLA ANUPAMA; NAGRE PRASHANT; TAMORE JAGDISH; PRABHU MANOJKUMAR SADANAND; KADAM SACHIN VASANT 权利人:FERMENTA BIOTECH LTD 摘要:Disclosed herein is an improved and efficient process for synthesis of vitamin D3 and its analogue Calcifediol from Ergosterol. Particularly, the present invention discloses the synthesis of key intermediate 3β-tert-Butyldimethylsilyloxy-22-hydroxy-23,24-bisnorchola-5,7-diene (5), and novel intermediate β-tert-Butyldimethylsilyloxy-22-iodo-23,24-bisnorchola-5,7-diene (9) by a simple and cost effective process. The industrially viable processes for preparation of said intermediate(s) results in providing provitamins with various side chains and the desired products in high yield.
专利号:US-5292977-A 优先权日:1992-02-05 标题:Palladium catalyzed alkylative cyclization useful in synthesis of vitamin D and analogues 发明人:TROST BARRY M; DUMAS JACQUES 权利人:UNIV LELAND STANFORD JUNIOR 摘要:An alkylative cycloaddition method is provided that is particularly useful for the synthesis of many of the Vitamin D analogues with differing side chains. Thus, a preferred synthesis is of Vitamin D analogues having a side chain R 1 where a substantially geometrically pure first precursor having the structure ##STR1## and a second precursor are provided, the second precursor being a 1,7 enyne. These precursors are reacted in the presence of a palladium catalyst to form compounds having the structure ##STR2## where R 2 hydrogen, hydroxyl, lower alkoxy, fluorine, or a protecting group, and R 3 is hydrogen, hydroxyl, lower alkoxy, fluorine, or a protecting group.
专利号:US-6844461-B2 优先权日:2001-07-30 标 题:Synthesis of A-ring synthon of 19-NOR-1α,25-dihydroxyvitamin D3 from (D)-glucose 发明人:DELUCA HECTOR F; SHIMIZU MASATO; YAMADA SACHIKO 权利人:WISCONSIN ALUMNI RES FOUND 摘要:The present invention provides a method for the synthesis of an A-ring synthon phosphine oxide used in the preparation of 19-nor vitamin D compounds, and to novel synthetic intermediates formed during the synthesis. The new method prepares the phosphine oxide from (D)-glucose.
专利号:US-4098801-A 优先权日:1977-01-26 标 题:Synthesis of 1α-hydroxylated derivatives of cholesterol 发明人:MICHELI ROBERT ANGELO 权利人:HOFFMANN LA ROCHE 摘要:A process for the preparation of 1α-hydroxylated cholesterol derivatives useful for the synthesis of 1α-hydroxylated cholecalciferols, is disclosed.
专利号:US-5352670-A 优先权日:1991-06-10 标题:Methods for the enzymatic synthesis of alpha-sialylated oligosaccharide glycosides 发明人:VENOT ANDRE P; UNGER FRANK M; KASHEM MOHAMMED A; BIRD PAUL; MAZID M ABDUL 权利人:ALBERTA RES COUNCIL 摘要:Disclosed are methods for the enzymatic synthesis of alpha-sialylated oligosaccharide glycosides. Specifically, in the disclosed methods, sialyltransferase is activated to transfer an analogue of sialic acid, employed as its CMP-nucleotide derivative, to an oligosaccharide glycoside. The analogue of sialic acid and the oligosaccharide employed in this method are selected to be compatible with the sialyltransferase employed.
专利号:US-5446225-A 优先权日:1992-02-05 标题:Palladium catalyzed akylative cyclization useful in syntheses of Vitamin D and analogues 发明人:TROST BARRY M; DUMAS JACQUES 权利人:UNIV LELAND STANFORD JUNIOR 摘要:An alkylative cycloaddition method is provided that is particularly useful for the synthesis of many of the Vitamin D analogues with differing side chains. Thus, a preferred synthesis is of Vitamin D analogues having a side chain R 1 where a first precursor having the structure ##STR1## with X being a halide or a pseudo halide, and a second precursor are provided, the second precursor being a 1,7 enyne. These precursors are reacted in the presence of a palladium catalyst to form compounds having the structure ##STR2## where R 2 is hydrogen, hydroxyl, lower alkoxy, fluorine, or a protecting group, and R 3 is hydrogen, hydroxyl, lower alkoxy, fluorine, or a protecting group.
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合成参考文献
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