公开(公告)号：US5089652A

公开(公告)日：1992-02-18

申请号：US466221

申请日：1990-01-17

Applicant: Joseph A. Sohara ,  Randal A. Johnson ,  William E. Gorton

Inventor： Joseph A. Sohara ,  Randal A. Johnson ,  William E. Gorton

IPC: C07C201/02 ,  C07C203/02 ,  C07C203/04

CPC classification number: C07C201/02

Abstract: The process of the present invention provides a method of obtaining a high yield of water or acid soluble nitrate esters without the use of organic solvents in the nitration reaction or the production of unstable products or by-products. The process involves the nitration of an organic hydroxy-containing compound with a suitable nitrating agent such as nitric acid in the absence of organic solvents in the nitration reaction. The reaction mixture is neutralized, causing the nitrate esters to precipitate or separate from the neutralized nitrate solution. The nitrate ester is then recovered, and any dissolved nitrate salts can be removed therefrom by gentle washing with water or a dilute halide solution. As provided by the process of the present invention, no organic solvents are used in the nitration reaction and average yields range from about 80% to about 95%.

Abstract translation: 本发明的方法提供了在硝化反应或不稳定产物或副产物的生产中不使用有机溶剂获得高产率的水或酸可溶性硝酸酯的方法。 该方法包括在硝化反应中在不存在有机溶剂的情况下用合适的硝化剂如硝酸硝化含有机羟基化合物。 将反应混合物中和，使硝酸酯从中和的硝酸盐溶液中沉淀或分离。 然后回收硝酸酯，通过用水或稀卤化物溶液温和洗涤可以将任何溶解的硝酸盐除去。 如本发明方法所提供的，在硝化反应中不使用有机溶剂，平均收率在约80％至约95％的范围内。

公开(公告)号：US4820859A

公开(公告)日：1989-04-11

申请号：US794340

申请日：1985-11-05

Applicant: Ross W. Millar ,  Norman C. Paul ,  David H. Richards

Inventor： Ross W. Millar ,  Norman C. Paul ,  David H. Richards

IPC: C07C201/02 ,  C07C203/04 ,  C08C19/40 ,  C07C77/02

CPC classification number: C08C19/40 ,  C07C201/02 ,  C07C243/02

Abstract: A process for the production of a high energy material involves reacting, in an inert organic solvent, a heterocyclic compound selected from oxirane, aziridine, oxetane or azetidine with a nitrogen oxide selected from dinitrogen tetroxide (N.sub.2 O.sub.4) and dinitrogen pentoxide (N.sub.2 O.sub.5) and, when the nitrogen oxide is N.sub.2 O.sub.4, oxidizing the O- or N- nitroso substituent or substituents in the product obtained to O- or N- nitro substituent or substituents. The heterocyclic compounds may be substituents or unsubstituted. In the former case the preferred substituents groups are halogen, alkyl, alkenyl, nitro and epoxy (as in epoxidized polybutadiene). The solvent is preferably a chlorinated alkane.Novel nitrated derivatives of polybutadiene, in which between 1% and 25% of the carbon atoms in the polymer are substituted by nitrate (ONO.sub.2), are also provided. These novel materials are liquid rubbers when the polybutadiene starting material has a molecular weight between 2000 and 10000.

Abstract translation: 用于生产高能材料的方法包括在惰性有机溶剂中使选自环氧乙烷，氮丙啶，氧杂环丁烷或氮杂环丁烷的杂环化合物与选自四氧化二氮（N 2 O 4）和五氧化二氮（N 2 O 5）的氮氧化物反应， 当氮氧化物是N 2 O 4时，将获得的产物中的O-或N-亚硝基取代基或取代基氧化成O-或N-硝基取代基。 杂环化合物可以是取代基或未取代的。 在前一种情况下，优选的取代基是卤素，烷基，烯基，硝基和环氧基（如在环氧化的聚丁二烯中）。 溶剂优选为氯化烷烃。 还提供了聚合物中1％至25％的碳原子被硝酸（ONO 2）取代的聚丁二烯的新型硝化衍生物。 当聚丁二烯起始材料的分子量在2000和10000之间时，这些新型材料是液体橡胶。

公开(公告)号：US4683323A

公开(公告)日：1987-07-28

申请号：US758801

申请日：1985-07-25

Applicant: Masayoshi Minai ,  Yuji Ueda

Inventor： Masayoshi Minai ,  Yuji Ueda

IPC: C07C45/64 ,  C07C45/67 ,  C07C49/707 ,  C07C203/08 ,  C07C309/63 ,  C07C143/68

CPC classification number: C07C201/02 ,  C07C303/28 ,  C07C45/64 ,  C07C45/673 ,  C07B2200/07 ,  C07C2101/08

Abstract: By hydrolyzing a sulfonic acid ester or a nitric acid ester of an optically active 4-hydroxy-2-cyclopentenone, the steric inversion of the hydroxyl group at the 4-position of the cyclopentenone mentioned above is effected.4-hydroxy-2-cyclopentenone is useful as a raw material of prostaglandins (natural substance is an (R)-substance) having stimulative action to uterine muscle and vasodilator action. For instance, 4(S)-hydroxy-2-cyclopentenone can be configurationally inverted to R-isomer. Accordingly, this method is extremely meaningful in the synthesis of prostaglandins.

Abstract translation: 通过水解光学活性的4-羟基-2-环戊烯酮的磺酸酯或硝酸酯，可以实现上述环戊烯酮在4-位的羟基的立体倒置。 4-羟基-2-环戊烯酮可用作具有对子宫肌肉和血管扩张剂作用的刺激作用的前列腺素（天然物质是（R））的原料。 例如，可以将4（S） - 羟基-2-环戊烯酮构型反转成R-异构体。 因此，这种方法在前列腺素的合成中是非常有意义的。

公开(公告)号：US4487988A

公开(公告)日：1984-12-11

申请号：US489466

申请日：1983-04-28

Applicant: Ian M. Campbell ,  Donald L. Baulch ,  Jonathan M. Chappel

Inventor： Ian M. Campbell ,  Donald L. Baulch ,  Jonathan M. Chappel

IPC: C07C201/02 ,  C07C201/04 ,  C07C201/08 ,  C07C203/00 ,  C07C203/02 ,  C07C205/02 ,  C07C76/02

CPC classification number: C07C201/04 ,  C07C201/02 ,  C07C201/08

Abstract: Organic nitrogen compounds are formed in the vapor phase by organic radical formation by reaction of an organic compound, suitably an alkane, with hydroxyl radicals derived from the reaction between hydrogen peroxide and nitrogen dioxide and the nitration of the organic radicals, suitably with nitrogen dioxide. The process is conducted using a molecular oxygen additive which directs the reaction towards the formation of the nitrate corresponding to the organic compound which may predominate in the organic reaction products.

Abstract translation: 通过有机化合物（合适的是烷烃）与由过氧化氢和二氧化氮之间的反应衍生的羟基自由基以及适当地用二氧化氮硝化有机自由基的有机自由基形成形成有机氮化合物。 该方法使用分子氧添加剂进行，该分子氧添加剂将反应引导形成对应于有机反应产物中可能占优势的有机化合物的硝酸盐。

公开(公告)号：US4047989A

公开(公告)日：1977-09-13

申请号：US687649

申请日：1976-05-18

Applicant: Sverre Ludvik Ostern

Inventor： Sverre Ludvik Ostern

IPC: C06B21/00 ,  C06B25/10 ,  C06B23/00

CPC classification number: C07C201/02 ,  C06B21/0091 ,  C06B25/10

Abstract: Blasting oil contained in the effluent from the production of explosives containing nitroglycerine is recovered by extracting with nitroaromatics which make part of the final explosive, the resulting extract being used completely in the explosive production. Residues of nitroaromatics may be removed from the purified effluent by means of an extraction liquid being sparely water-soluble, such as toluene or xylene or a mixture thereof.

Abstract translation: 含有硝酸甘油的爆炸物生产的废液中含有的爆炸油通过用作为最终爆炸物的一部分的硝基芳族化合物提取而回收，所得提取物完全用于爆炸生产。 硝基芳族化合物的残留物可以通过无水溶性的萃取液如甲苯或二甲苯或其混合物从纯化的流出物中除去。

公开(公告)号：US3450742A

公开(公告)日：1969-06-17

申请号：US3450742D

申请日：1958-11-03

Applicant: ROHM & HAAS

Inventor： EMMONS WILLIAM D ,  ROLEWICZ HENRY A

IPC: C06B21/00 ,  C06B45/10 ,  C07C203/04 ,  C07C77/02 ,  C06B3/00

CPC classification number: C06B45/105 ,  C06B21/0008 ,  C07C201/02 ,  C07C203/04

公开(公告)号：US3420869A

公开(公告)日：1969-01-07

申请号：US3420869D

申请日：1967-04-13

Applicant: US INTERIOR

Inventor： WEKELL JOHN C ,  HOULE CLIFFORD R ,  MALINS DONALD C

IPC: C07C203/04 ,  C07C203/08 ,  C07C77/02

CPC classification number: C07C201/02 ,  C07C203/04 ,  C07C2603/40 ,  C07C203/10 ,  C07C203/08

公开(公告)号：US3409620A

公开(公告)日：1968-11-05

申请号：US62933667

申请日：1967-02-06

Applicant: MARIO BIAZZI SA DR ING

Inventor： VALTER OHMAN PER ,  HANSPETER MOSER

IPC: B01J3/00 ,  B01J19/18 ,  C07B43/02 ,  C07C201/02 ,  C07C201/08 ,  C07C201/12 ,  C07C203/04 ,  C07C205/06

CPC classification number: B01J3/006 ,  B01J19/18 ,  B01J2219/00063 ,  B01J2219/00123 ,  B01J2219/00128 ,  B01J2219/00164 ,  B01J2219/00177 ,  B01J2219/185 ,  C07B43/02 ,  C07C201/02 ,  C07C201/08 ,  C07C203/04 ,  C07C205/06

公开(公告)号：US3408383A

公开(公告)日：1968-10-29

申请号：US64495757

申请日：1957-03-08

Applicant: ROHM & HAAS

Inventor： ROLEWICZ HENRY A ,  GRIMES JR CHARLES D ,  STEVENSON JR KENYON

IPC: C07C203/04

CPC classification number: C07C201/02 ,  C07C203/04

公开(公告)号：US3301891A

公开(公告)日：1967-01-31

申请号：US64033457

申请日：1957-02-15

Applicant: BASF AG

Inventor： VON SCHICKH OTTO

IPC: C07C201/02

CPC classification number: C07C203/08 ,  C07C201/02 ,  C07C2601/14 ,  C07C2601/18

Abstract: Cycloaliphatic nitrates are produced by dissolving cycloaliphatic alcohols in an indifferent solvent and then treating them in this solution with nitrating acid. A suitable temperature range for the reaction is between +20 DEG and -40 DEG C., preferably between -5 DEG and -10 DEG C. Suitable cycloaliphatic alcohols are cyclopentanol, cyclohexanol, cyclo-octanol, cyclodecanol, decahydronaphthol, the isomers of methyl cyclohexanol and dimethylcyclohexanol and mixtures of such alcohols. Examples of indifferent solvents are aliphatic halogenated hydrocarbons, such as chloroform, carbon tetrachloride and ethylene chloride, or aliphatic hydrocarbons, such as petroleum ether, hexane, or heptane, or cyclic hydrocarbons, such as methylcyclopentane, cyclohexane, methylcyclohexane, dimethyl cyclohexane or mixtures thereof. The alcohol is dissolved in the solvent in a ratio of 1 part alcohol to 1, 2, 3 or more parts of solvent. The nitrating acid is a mixture of 1 part of concentrated nitric acid to 1, 2, 3 or more parts of concentrated sulphuric acid. The nitration may be carried out continuously by leading the reactants through a tubular coil at the desired temperature. In examples: (1) cyclohexanol dissolved in carbon tetrachloride is introduced rapidly with stirring into a nitrating acid mixture cooled to -5 DEG to -10 DEG C., and the organic layer is washed with water and soda solution and fractionally distilled to obtain cyclohexanol nitrate; methylcyclohexanol nitrate and dimethylcyclohexanol nitrate are similarly obtained; (2) cyclopentanol dissolved in chloroform is nitrated as in (1) and poured on to crushed ice, the organic layer is washed with sodium bisulphite to remove cyclopentanone, then with water and soda and then is fractionally distilled to obtain cyclopentanol nitrate; cyclo-octanol nitrate is similarly obtained; (3) decahydronaphthol nitrate is obtained by the process of (1). The products are valuable fuel additives.