CAS: 6303-21-5; Hypophosphorous Acid

上下游产品

water phosphan sulphurous acid phosphonic Acidcerium orthophosphate ammonium hypophosphorous acid 2-(3,5-dichlorophenyl)acetaldehyde 5-bromo-2-tert-butyl-1-[(4'-methyl)phenoxy]benzene

Sodium Hypophosphite置于盐酸体系中,用 甲苯 作为反应溶剂,以83%的收率获得产物次磷酸
参考文献:镍催化次磷酸钠参与炔烃直接氢化磷酸化反应生成 H-次膦酸盐
标题:镍催化次磷酸钠参与炔烃直接氢化磷酸化反应生成 H-次膦酸盐
摘要:传统的亚膦酸酯合成方法使用三氯化磷 (Pcl 3) 作为磷源,导致过程污染严重且能源密集.寻找一种既温和又环保的替代方法是现代化学中一项具有挑战性但回报丰厚的任务.在此,我们使用无机含磷物质 Nah 2 Po 2作为磷源,直接参与镍催化的选择性炔烃氢膦酰化反应.这种转变是在室温下以多组分方式实现的,最重要的是,H-反应生成的次膦酸盐产品是一种高级中间体,可以很容易地转化为多种次膦酸盐衍生物,包括带有新 P-C,P-S,P-N,P-Se 和 P-O 键的衍生物,从而提供一种补充方法经典的次膦酸酯合成技术.
DOI:10.1021/acs.Joc.2C02741

专利信息

专利号:EP-1634887-A3
优先权日:2004-07-23
标题 :Process for synthesis of complex 2-deoxy-2-iodo pyranosides of high purity, particularly suitable for manufacturing pharmaceutically pure annamycin
发明人：SZEJA WIESLAW; FOKT IZABELA; GRYNKIEWICZ GRZEGORZ
权利人:ZAKLAD BADAWCZO PROD
摘要:The method according to the invention comprises using as glycosyl donors high purity 2-deoxy-2-iodo derivatives of sugars of a defined configuration of C-2 carbon with O-alkyl, S-alkyl, O-aryl, S-aryl, O-heteroaryl, S-heteroaryl, O-acyl, O-silyl, O-N-imido, O-P-(phosphino, phosphono, thiophosphono, selenophosphono) groups at the anomeric position, and subjecting them to a condensation reaction with a compound containing a hydroxyl group or a protected hydroxyl group in the presence of electrophilic reagents, followed by deprotection and isolation of a pharmaceutically pure product. The objective of the present invention is to provide a method for preparing complex glycosides by coupling cyclic multifunctional compounds containing hydroxyl functional groups (glycosyl acceptors, including aglycones of natural origin which are known as constituents of active pharmaceutical ingredients) with diastereoisomerically pure 2-deoxy-2-halopyranosyl derivatives containing anomeric substituent capable of exchange under glycosidating conditions, for example by virtue of activation with electrophilic agents. This method substantially simplifies the synthesis of Annamycin. n The present invention relies on a regio- and stereoselective reaction of cohalogenating 1,2-unsaturated sugars in the presence of hydroxyl group containing compounds, such as: water, alcohols, phenols, carboxylic acids, silanols, phosphinic acids, phosphoric acids, thiophosphoric acids, selenophosphoric acids, followed by separation of the product with proper C-2 carbon configuration required for the synthesis. As the separation of stereoisomers is carried out at the stage of obtaining a relatively inexpensive intermediate in the form of glycosyl donor, the method of the invention substantially reduces the cost of Annamycin manufacture. Other advantages of the synthesis process of the invention consist in the reduction of the number of stages of the antibiotic manufacture process and in yield increase of the final product.

专利号:US-7241399-B2
优先权日:2000-09-08
标题 :Synthesis of nanoparticles
发明人：HAUBOLD STEPHAN; HAASE MARKUS; RIWOTZKI KARSTEN; WELLER HORST; MEYSSAMY HEIKE; IBARRA FERNANDO
权利人:CT ANGEWANDTE NANOTECH CAN
摘要:Methods for the preparation of inorganic nanoparticles capable of fluorescence, wherein the nanoparticles consist of a host material that comprises at least one dopant. The synthesis of the invention in organic solvents allows to gain a considerably higher yield compared to the prior art synthesis in water. All kinds of objects can advantageously be marked and reliably authenticated by using an automated method on the basis of a characteristic emission. Further, the size distribution of the prepared nanoparticles is nartower which renders a subsequent size-selected separation process superfluous.

专利号:WO-2007003236-A1
优先权日:2005-06-30
标 题:Process for synthesis of complex 2-deoxy-2-iodo pyranosides of high purity, particularly suitable for manufacturing pharmaceutically pure annamycin
发明人：SZEJA WIESLAW; GRYNKIEWICZ GRZEGORZ; FOKT IZABELA
权利人:ZACLAD BADAWCZO PROD SYNTEX; SZEJA WIESLAW; GRYNKIEWICZ GRZEGORZ; FOKT IZABELA
摘要:The method according to the invention comprises using as glycosyl donors high purity 2- deoxy-2-iodo derivatives of sugars of a defined configuration of C-2 carbon with O-alkyl, S- alkyl, O-aryl, S-aryl, O-heteroaryl, S-heteroaryl, O-acyl, O-silyl, O-N-imido, O-P- (phosphino, phosphono, thiophosphono, selenophosphono) groups at the anomeric position, and subjecting them to a condensation reaction with a compound containing a hydroxyl group or a protected hydroxyl group in the presence of electrophilic reagents, followed by deprotection and isolation of a pharmaceutically pure product. The objective of the present invention is to provide a method for preparing complex glycosides by coupling cyclic multifunctional compounds containing hydroxyl functional groups (glycosyl acceptors, including aglycones of natural origin which are known as constituents of active pharmaceutical ingredients) with diastereoisomerically pure 2-deoxy-2-halopyranosyl derivatives containing anomeric substituent capable of exchange under glycosidating conditions, for example by virtue of activation with electrophilic agents. This method substantially simplifies the synthesis of Annamycin. The present invention relies on a regio- and stereoselective reaction of cohalogenating 1,2- unsaturated sugars in the presence of hydroxyl group containing compounds, such as: water, alcohols, phenols, carboxylic acids, silanols, phosphinic acids, phosphoric acids, thiophosphoric acids, selenophosphoric acids, followed by separation of the product with proper C-2 carbon configuration required for the synthesis. As the separation of stereoisomers is carried out at the stage of obtaining a relatively inexpensive intermediate in the form of glycosyl donor, the method of the invention substantially reduces the cost of Annamycin manufacture. Other advantages of the synthesis process of the invention consist in the reduction of the number of stages of the antibiotic manufacture process and in yield increase of the final product.

专利号:US-3956184-A
优先权日:1974-04-24
标题:Method of preparing silver catalyst for synthesis of formaldehyde by oxidizing methyl alcohol
发明人：KRUGLIKOV ANATOLY ABRAMOVICH; YAKOVENKO ZEMFIRA IVANOVNA; ROZNINA MARINA IVANOVNA; ROGACHEVA ANNA MALOFEEVNA; BELOUSOV GERMAN IVANOVICH
权利人:KRUGLIKOV ANATOLY ABRAMOVICH; YAKOVENKO ZEMFIRA IVANOVNA; ROZNINA MARINA IVANOVNA; ROGACHEVA ANNA MALOFEEVNA; BELOUSOV GERMAN IVANOVICH
摘要:The method of preparing a silver catalyst for synthesis of formaldehyde by oxidizing methyl alcohol which consists in that a carrier is impregnated with an aqueous or an aqueous-alcohol solution containing complex ions of silver having the general formula [Ag(X) n ] + or [Ag(Y) 2 ] - , where X is ammonia, ethylenediamine, triethylenetetramine or triaminotriethylamine, Y is a thiocyanate, cyanide, acetate, or hydroxyl ion, and n is 1 or 2. The impregnated carrier is processed, at a temperature of from 10° - 100°C, with a reducing agent taken in the quantity sufficient to reduce the silver completely from said ion. The thus-prepared catalyst is dried at a temperature of from 80° to 400°C. It is recommended that the catalyst be washed with water before drying. The thus-prepared catalyst has a highly developed active surface with a small content of silver (the specific surface of the catalyst is 0.7 - 7 square meters per gram, with the metal silver content of the catalyst being from 5 - 10 per cent by weight). The catalyst is highly active and has good selectivity in the process of formaldehyde synthesis from methyl alcohol. The yield of formaldehyde with the proposed catalyst is from 75 - 80 per cent, calculating with reference to the passed methyl alcohol, with the selectivity of the process being from 89 - 95 per cent.

专利号:US-9051516-B2
优先权日:2011-11-16
标 题:Melt stabilization and vapor-phase synthesis of cesium germanium halides
发明人：BOWMAN STEVEN R; CONDON NICHOLAS J; O'CONNOR SHAWN P
权利人:US NAVY
摘要:The method described herein allows for melt stabilization and vapor-phase synthesis of a cesium germanium halide utilizing germanium dihalides formed in situ. This disclosure allows for the melting of cesium germanium halides without decomposition, which allows for growing crystals of these materials from the melt. This disclosure allows for a direct synthesis of these materials without the use of water or the introduction of other possible contaminants.

专利号:US-8735586-B2
优先权日:2007-06-26
标 题 :Regioselective copper catalyzed synthesis of benzimidazoles and azabenzimidazoles
发明人：ALONSO JORGE; LINDENSCHMIDT ANDREAS; NAZARÉ MARC; URMANN MATTHIAS; HALLAND NIS; RKYEK OMAR
权利人:ALONSO JORGE; LINDENSCHMIDT ANDREAS; NAZARÉ MARC; URMANN MATTHIAS; HALLAND NIS; RKYEK OMAR; SANOFI SA
摘要:The present invention relates to a process for the regioselective synthesis of compounds of the formula I, n nwherein R0; R1; R2; R3; R4; R5; A1; A2; A3; A4, Q and J have the meanings indicated in the claims. The present invention provides a direct copper catalyzed regioselective process to a wide variety of unsymmetrical, multifunctional N-substituted benzimidazoles or azabenzimidazoles of formula I starting from 2-halo-nitroarenes and N-substituted amides.