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1. 发明授权

US07057072B2 Synthesis and purification of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) 失效
标题翻译： 1,3,5-三氨基-2,4,6-三硝基苯（TATB）的合成与纯化
公开(公告)号：US07057072B2
公开(公告)日：2006-06-06
申请号：US10910659
申请日：2004-08-02
申请人： Alexander R. Mitchell , Michael D. Coburn , Gregory S. Lee , Robert D. Schmidt , Philip F. Pagoria , Peter C. Hsu
发明人： Alexander R. Mitchell , Michael D. Coburn , Gregory S. Lee , Robert D. Schmidt , Philip F. Pagoria , Peter C. Hsu
IPC分类号： C07C209/18 , C07C211/50 , C07C209/84
CPC分类号： C06B25/04 , C06B21/0091 , C07C211/52
摘要： A method to convert surplus nitroarene explosives (picric acid, ammonium picrate,) into TATB is described. The process comprises three major steps: conversion of picric acid/ammonium picrate into picramide; conversion of picramide to TATB through vicarious nucleophilic substitution (VNS) of hydrogen chemistry; and purification of TATB.
摘要翻译：描述了将过量的硝基芳烃炸药（苦味酸，苦味酸铵）转化成TATB的方法。该方法包括三个主要步骤：将苦味酸/苦味酸铵转化成草甘膦; 通过氢化学的替代亲核取代（VNS）将picramide转化为TATB; 和TATB的纯化。

2. 发明授权

US07057073B2 Synthesis of trinitrophloroglucinol and triaminotrinitrobenzene (TATB) 失效
标题翻译：三硝基间苯三酚和三氨基硝基苯（TATB）的合成
公开(公告)号：US07057073B2
公开(公告)日：2006-06-06
申请号：US10912723
申请日：2004-08-04
申请人： Alexander R. Mitchell , Michael D. Coburn , Gregory S. Lee , Robert D. Schmidt , Philip F. Pagoria , Peter C. Hsu
发明人： Alexander R. Mitchell , Michael D. Coburn , Gregory S. Lee , Robert D. Schmidt , Philip F. Pagoria , Peter C. Hsu
IPC分类号： C07C209/18 , C07C211/50 , C07C205/06
CPC分类号： C07C201/06 , C07C209/18 , C07C211/52 , C07C205/24
摘要： A method to convert surplus nitroarene explosives into trinitrophloroglucinol and triaminotrinitrobenzene (TATB) is described. Picric acid is directly aminated to diaminopicric acid, which is converted to trinitrophloroglucinol and triaminotrinitrobenzene.
摘要翻译：描述了将多余的硝基芳烃炸药转化为三硝基间苯三酚和三氨基硝基苯（TATB）的方法。苦草酸直接胺化成二氨基酸，转化为三硝基间苯三酚和三氨基硝基苯。

3. 发明授权

US5633406A Vicarious nucleophilic substitution using 4-amino-1,2,4-triazole, hydroxylamine or O-alkylhydroxylamine to prepare 1,3-diamino-2,4,6-trinitrobenzene or 1,3,5-triamino-2,4,6-trinitrobenzene 失效
标题翻译：使用4-氨基-1,2,4-三唑，羟胺或O-烷基羟胺代替亲核取代，制备1,3-二氨基-2,4,6-三硝基苯或1,3,5-三氨基-2,4,6 - 二硝基苯
公开(公告)号：US5633406A
公开(公告)日：1997-05-27
申请号：US440024
申请日：1995-05-12
申请人： Alexander R. Mitchell , Philip F. Pagoria , Robert D. Schmidt
发明人： Alexander R. Mitchell , Philip F. Pagoria , Robert D. Schmidt
IPC分类号： C07C209/02
CPC分类号： C07C209/02
摘要： The present invention relates to a process to produce 1,3-diamino-2,4,6-trinitrobenzene (DATB) or 1,3,5-triamino-2,4,6,-trinitrobenzene (TATB) by:(a) reacting at ambient pressure and a temperature of between about 0.degree. and 50.degree. C. for between about 0.1 and 24 hr, a trinitroaromatic compound of structure V: ##STR1## wherein X, Y, and Z are each independently selected from the group consisting of --H and --NH.sub.2, with the proviso that at least 1 or 2 of X, Y, and Z are hydrogen;with an effective amount of 1-amino-1,2,4-triazole, hydroxylamine or O-alkylhydroxamine to produce DATB or TATB;in the presence of a strong base selected from sodium butoxide, potassium butoxide, potassium propoxide, sodium propoxide, sodium ethoxide, potassium ethoxide, sodium methoxide, potassium methoxide, and combinations thereof;in a solvent selected from the group consisting of methanol, ethanol, propanol, butanol, dimethylsulphoxide, N-methylpyrrolidone, hexamethylphosphoramide, dimethylformide, dimethylacetamide and mixtures thereof, provided that when alcohols are present or when hydroxylamine or its O-alkyl derivatives replace ATA primarily DATB is formed; and (b) isolating the DATB or TATB produced. DATB and TATB are important and useful specialty explosives and intermediates for other materials.
摘要翻译：本发明涉及通过以下方法制备1,3-二氨基-2,4,6-三硝基苯（DATB）或1,3,5-三氨基-2,4,6-三硝基苯（TATB）的方法：（a）在环境压力和约0℃至50℃的温度下反应约0.1至24小时，结构V的三硝基芳族化合物：其中X，Y和Z各自独立地选自由-H和-NH2组成的组，条件是X，Y和Z中至少有1或2个是氢; 与有效量的1-氨基-1,2,4-三唑，羟胺或O-烷基羟胺反应生成DATB或TATB; 在选自丁醇钠，丁醇钾，丙醇钾，丙醇钠，乙醇钠，乙醇钾，甲醇钠，甲醇钾及其组合的强碱的存在下，在选自甲醇，乙醇，丙醇，丁醇，二甲基亚砜，N-甲基吡咯烷酮，六甲基磷酰胺，二甲基甲酰胺，二甲基乙酰胺及其混合物的溶剂中，条件是当存在醇时或当羟胺或其O-烷基衍生物主要代替ATA时 DATB形成; 和（b）分离产生的DATB或TATB。 DATB和TATB是其他材料的重要和有用的特种炸药和中间体。

4. 发明授权

US6069277A Amination of electrophilic aromatic compounds by vicarious nucleophilic substitution 失效
标题翻译：通过亲核取代替代亲电芳族化合物
公开(公告)号：US6069277A
公开(公告)日：2000-05-30
申请号：US967914
申请日：1997-11-12
申请人： Alexander R. Mitchell , Philip F. Pagoria , Robert D. Schmidt
发明人： Alexander R. Mitchell , Philip F. Pagoria , Robert D. Schmidt
IPC分类号： C07C209/02 , C07C211/52 , C07C213/02 , C07C253/30
CPC分类号： C07C253/30 , C07C209/02 , C07C211/52 , C07C213/02
摘要： The present invention relates to a process to aminate electrophilic aromatic compounds by vicarious nucleophilic substitution of hydrogen using quaternary hydrazinium salts. The use of trialkylhydrazinium halide, e.g., trimethylhydrazinium iodide, as well as hydroxylamine, alkoxylamines, and 4-amino-1,2,4-triazole to produce aminated aromatic structures, such as 1,3-diamino-2,4,6-trinitrobenzene (DATB), 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) and 3,5-diamino-2,4,6-trinitrotoluene (DATNT), is described. DATB and TATB are useful insensitive high explosives. TATB is also used for the preparation of benzenehexamine, a starting material for the synthesis of novel materials (optical imaging devices, liquid crystals, ferromagnetic compounds).
摘要翻译：本发明涉及通过使用季ium盐代替氢亲核取代氨基化亲电芳族化合物的方法。使用三烷基肼鎓卤化物，例如三甲基碘化铵，以及羟胺，烷氧基胺和4-氨基-1,2,4-三唑来制备胺化的芳族结构，例如1,3-二氨基-2,4,6-三三硝基苯（DATB），1,3,5-三氨基-2,4,6-三硝基苯（TATB）和3,5-二氨基-2,4,6-三硝基甲苯（DATNT）。 DATB和TATB是有用的不敏感的高爆炸物。 TATB也用于制备苯六胺，一种用于合成新材料的原料（光学成像装置，液晶，铁磁性化合物）。

5. 发明授权

US5569783A Vicarious nucleophilic substitution to prepare 1,3-diamino-2,4,6-trinitrobenzene or 1,3,5-triamino-2,4,6-trinitrobenzene 失效
标题翻译：代替亲核取代制备1,3-二氨基-2,4,6-三硝基苯或1,3,5-三氨基-2,4,6-三硝基苯
公开(公告)号：US5569783A
公开(公告)日：1996-10-29
申请号：US440017
申请日：1995-05-12
申请人： Alexander R. Mitchell , Philip F. Pagoria , Robert D. Schmidt
发明人： Alexander R. Mitchell , Philip F. Pagoria , Robert D. Schmidt
IPC分类号： C07C209/02 , C07C211/52 , C07C213/02 , C07C253/30 , C07C45/00
CPC分类号： C07C209/02 , C07C211/52 , C07C213/02 , C07C253/30 , Y10T74/1956
摘要： The present invention relates to a process to produce 1,3-diamino-2,4,6-trinitrobenzene (DATB) or 1,3,5-triamino-2,4,6,-trinitrobenzene (TATB) by:(a) reacting at ambient pressure and a temperature of between about 0.degree. and 50.degree. C. for between about 0.1 and 24 hr, a trinitroaromatic compound of structure V: ##STR1## wherein X, Y, and Z are each independently selected from --H, or --NH.sub.2, with the proviso that at least 1 or 2 of X, Y, and Z are hydrogen,with an amount effective to produce DATB or TATB of 1,1,1-trialkylhydrazinium halide wherein alkyl is selected from methyl, ethyl, propyl or butyl and halide is selected from chloride, bromide or iodide.in the presence of a strong base selected from sodium butoxide, potassium butoxide, potassium propoxide, sodium propoxide, sodium ethoxide, potassium ethoxide, sodium methoxide, potassium methoxide, and combinations thereof;in a solvent selected from the group consisting of methanol, ethanol, propanol, butanol, dimethylsulphoxide, N-methylpyrrolidone, hexamethylphosphoramide, dimethylformide, dimethylacetamide and mixtures thereof, provided that when alcohols are present primarily DATB and picramide is formed; and (b) isolating the DATB or TATB produced. DATB and TATB are useful specialty explosives. TATB is also used for the preparation of benzenehexamine, a starting material for the synthesis of novel materials (optical imaging devices, liquid crystals, ferromagnetic compounds).
摘要翻译：本发明涉及通过以下方法制备1,3-二氨基-2,4,6-三硝基苯（DATB）或1,3,5-三氨基-2,4,6-三硝基苯（TATB）的方法：（a）在环境压力和约0℃至50℃的温度下反应约0.1至24小时，结构V的三硝基芳族化合物：其中X，Y和Z各自独立地选自 -H或-NH 2，条件是X，Y和Z的至少1或2个是氢，具有有效产生1,1,1-三烷基卤化腙的DATB或TATB的量，其中烷基选自甲基，乙基，丙基或丁基，卤化物选自氯化物，溴化物或碘化物。在选自丁醇钠，丁醇钾，丙醇钾，丙醇钠，乙醇钠，乙醇钾，甲醇钠，甲醇钾及其组合的强碱的存在下，在选自甲醇，乙醇，丙醇，丁醇，二甲基亚砜，N-甲基吡咯烷酮，六甲基磷酰胺，二甲基甲酰胺，二甲基乙酰胺及其混合物的溶剂中，条件是当主要存在醇主要为DATB和形成策马瑞明时; 和（b）分离产生的DATB或TATB。 DATB和TATB是有用的特种炸药。 TATB也用于制备苯六胺，一种用于合成新材料的原料（光学成像装置，液晶，铁磁性化合物）。

6. 发明授权

US08815606B2 Thin-layer chromatography and colorimetric analysis of multi-component explosive mixtures 有权
标题翻译：多组分爆炸性混合物的薄层色谱和比色分析
公开(公告)号：US08815606B2
公开(公告)日：2014-08-26
申请号：US12106400
申请日：2008-04-21
申请人： Philip F. Pagoria , Alexander R. Mitchell , Richard E. Whipple , M. Leslie Carman
发明人： Philip F. Pagoria , Alexander R. Mitchell , Richard E. Whipple , M. Leslie Carman
IPC分类号： G01N30/90 , G01N30/96
CPC分类号： G01N30/94 , G01N30/90 , G01N33/22
摘要： A thin-layer chromatography method for detection and identification of common military and peroxide explosives in samples includes the steps of provide a reverse-phase thin-layer chromatography plate; prepare the plate by marking spots on which to deposit the samples by touching the plate with a marker; spot one micro liter of a first standard onto one of the spots, spot one micro liter of a second standard onto another of the spots, and spot samples onto other of spots producing a spotted plate; add eluent to a developing chamber; add the spotted plate to the developing chamber; remove the spotted plate from the developing chamber producing a developed plate; place the developed plate in an ultraviolet light box; add a visualization agent to a dip tank; dip the developed plate in the dip tank and remove the developed plate quickly; and detect explosives by viewing said developed plate.
摘要翻译：用于检测和鉴定样品中常见的军用和过氧化物炸药的薄层色谱法包括提供反相薄层色谱板的步骤; 通过用标记触摸板来标记沉积样品的斑点来准备板; 将一微升第一标准物放在其中一个斑点上，将一微升第二标准物放在另一个斑点上，并将样品点样到产生斑点板的其他斑点上; 将洗脱液加入显影室; 将点样板加到显影室; 从显影室中取出点样板，产生显影板; 将显影的板放在紫外灯箱中; 将一个可视化代理添加到浸槽中; 将显影的板块浸入浸渍槽中，快速取出显影板; 并通过查看所述显影板来检测爆炸物。

7. 发明申请

US20090299067A1 New synthesis of 2,6-diamino-3,5-dinitropyrazine-1-oxide from 2,6-diaminopyrazine-1-oxide 审中-公开
标题翻译： 2,6-二氨基吡嗪-1-氧化物新合成2,6-二氨基-3,5-二硝基吡嗪-1-氧化物
公开(公告)号：US20090299067A1
公开(公告)日：2009-12-03
申请号：US12130444
申请日：2008-05-30
申请人： Philip F. Pagoria , Alexander R. Mitchell , Kason Bala
发明人： Philip F. Pagoria , Alexander R. Mitchell , Kason Bala
IPC分类号： C07D241/20
CPC分类号： C07D241/20
摘要： A method for the synthesis of 2,6-Diamino-3,5-dinitropyrazine-1-oxide including nitration of 2,6-diaminopyrazine-1-oxide. The step of nitration may use nitrating agents 20% Oleum/100% HNO3, 100% HNO3 and conc. H2504/100% HNO3 or nitronium tetrfluoraoborate. The synthesis of 2,6-diaminopyrazine-1-oxide may involve both the oxidation of 2,6-diaminopyrazine, the amination of a precursor 2,6-disubstitutedpyrazine-1-oxide or direct formation of the 2,6-diaminopyrazine-l-oxide from the precursor, 2-amino-6-hydroxamino-pyrazine-1-oxide.
摘要翻译：合成2,6-二氨基-3,5-二硝基吡嗪-1-氧化物的方法，包括2,6-二氨基吡嗪-1-氧化物的硝化。硝化步骤可以使用硝化剂20％油/ 100％HNO 3，100％HNO 3和浓度。 H2504 / 100％HNO3或硝基四氟硼酸盐。 2,6-二氨基吡嗪-1-氧化物的合成可能涉及2,6-二氨基吡嗪的氧化，前体2,6-二取代吡嗪-1-氧化物的胺化或直接形成2,6-二氨基吡嗪-1 氧化物，2-氨基-6-羟基 - 吡嗪-1-氧化物。

8. 发明申请

US20090068065A1 Simple, Field Portable Colorimetric Detection Device For Organic Peroxides and Hydrogen Peroxide 有权
标题翻译：用于有机过氧化物和过氧化氢的简单现场便携式比色检测装置
公开(公告)号：US20090068065A1
公开(公告)日：2009-03-12
申请号：US12183210
申请日：2008-07-31
申请人： Philip F. Pagoria , Alexander R. Mitchell , Richard E. Whipple , M. Leslie Carman , John G. Reynolds , Peter Nunes , Sharon J. Shields
发明人： Philip F. Pagoria , Alexander R. Mitchell , Richard E. Whipple , M. Leslie Carman , John G. Reynolds , Peter Nunes , Sharon J. Shields
IPC分类号： G01N21/00 , B23P11/00
CPC分类号： G01N21/78 , G01N31/228 , Y10T29/49826 , Y10T436/206664
摘要： A simple and effective system for the calorimetric determination of organic peroxides and hydrogen peroxide. A peroxide pen utilizing a swipe material attached to a polyethylene tube contains two crushable vials. The two crushable vials contain a calorimetric reagent separated into dry ingredients and liquid ingredients. After swiping a suspected substance or surface the vials are broken, the reagent is mixed thoroughly and the reagent is allowed to wick into the swipe material. The presence of organic peroxides or hydrogen peroxide is confirmed by a deep blue color.
摘要翻译：有机过氧化物和过氧化氢的量热测定的简单而有效的系统。使用连接到聚乙烯管上的滑动材料的过氧化物笔包含两个可压碎的小瓶。两个可压碎的小瓶含有分配成干成分和液体成分的量热试剂。打扫怀疑的物质或表面后，小瓶破裂，将试剂充分混合，使试剂吸入滑动材料。有机过氧化物或过氧化氢的存在通过深蓝色证实。

9. 发明授权

US07829020B2 Simple, field portable colorimetric detection device for organic peroxides and hydrogen peroxide 有权
标题翻译：简单的现场便携式比色检测装置，用于有机过氧化物和过氧化氢
公开(公告)号：US07829020B2
公开(公告)日：2010-11-09
申请号：US12183210
申请日：2008-07-31
申请人： Philip F. Pagoria , Alexander R. Mitchell , Richard E. Whipple , M. Leslie Carman , John G. Reynolds , Peter Nunes , Sharon J. Shields
发明人： Philip F. Pagoria , Alexander R. Mitchell , Richard E. Whipple , M. Leslie Carman , John G. Reynolds , Peter Nunes , Sharon J. Shields
IPC分类号： G01N33/22
CPC分类号： G01N21/78 , G01N31/228 , Y10T29/49826 , Y10T436/206664
摘要： A simple and effective system for the colorimetric determination of organic peroxides and hydrogen peroxide. A peroxide pen utilizing a swipe material attached to a polyethylene tube contains two crushable vials. The two crushable vials contain a colorimetric reagent separated into dry ingredients and liquid ingredients. After swiping a suspected substance or surface the vials are broken, the reagent is mixed thoroughly and the reagent is allowed to wick into the swipe material. The presence of organic peroxides or hydrogen peroxide is confirmed by a deep blue color.
摘要翻译：用于比色测定有机过氧化物和过氧化氢的简单而有效的系统。使用连接到聚乙烯管上的滑动材料的过氧化物笔包含两个可压碎的小瓶。两个可压碎的小瓶包含分离成干成分和液体成分的比色试剂。打扫怀疑的物质或表面后，小瓶破裂，将试剂充分混合，使试剂吸入滑动材料。有机过氧化物或过氧化氢的存在通过深蓝色证实。

10. 发明申请

US20090221085A1 Thin-Layer Chromatography and Colorimetric Analysis of Multi-Component Explosive Mixtures 有权
标题翻译：多组分爆炸混合物的薄层色谱和比色分析
公开(公告)号：US20090221085A1
公开(公告)日：2009-09-03
申请号：US12106400
申请日：2008-04-21
申请人： Philip F. Pagoria , Alexander R. Mitchell , Richard E. Whipple , M. Leslie Carman
发明人： Philip F. Pagoria , Alexander R. Mitchell , Richard E. Whipple , M. Leslie Carman
IPC分类号： G01N30/90
CPC分类号： G01N30/94 , G01N30/90 , G01N33/22
摘要： A thin-layer chromatography method for detection and identification of common military and peroxide explosives in samples includes the steps of provide a reverse-phase thin-layer chromatography plate; prepare the plate by marking spots on which to deposit the samples by touching the plate with a marker; spot one micro liter of a first standard onto one of the spots, spot one micro liter of a second standard onto another of the spots, and spot samples onto other of spots producing a spotted plate; add eluent to a developing chamber; add the spotted plate to the developing chamber; remove the spotted plate from the developing chamber producing a developed plate; place the developed plate in an ultraviolet light box; add a visualization agent to a dip tank; dip the developed plate in the dip tank and remove the developed plate quickly; and detect explosives by viewing said developed plate.
摘要翻译：用于检测和鉴定样品中常见的军用和过氧化物炸药的薄层色谱法包括提供反相薄层色谱板的步骤; 通过用标记触摸板来标记沉积样品的斑点来准备板; 将一微升第一标准物放在其中一个斑点上，将一微升第二标准物放在另一个斑点上，并将样品点样到产生斑点板的其他斑点上; 将洗脱液加入显影室; 将点样板加到显影室; 从显影室中取出点样板，产生显影板; 将显影的板放在紫外灯箱中; 将一个可视化代理添加到浸槽中; 将显影的板块浸入浸渍槽中，快速取出显影板; 并通过查看所述显影板来检测爆炸物。

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