RU2010140375A - METHOD FOR PRODUCING CRYSTALLINE 2,4,6,8,10,12-HEXANITRO-2,4,6,8,10,12-HEXAAZATETRACYCLO [5,5,03,11,05,9] DODECAN WITH PRESENT POLYMORPHIC COMPOSITION (OPTIONS ) - Google Patents
METHOD FOR PRODUCING CRYSTALLINE 2,4,6,8,10,12-HEXANITRO-2,4,6,8,10,12-HEXAAZATETRACYCLO [5,5,03,11,05,9] DODECAN WITH PRESENT POLYMORPHIC COMPOSITION (OPTIONS ) Download PDFInfo
- Publication number
- RU2010140375A RU2010140375A RU2010140375/04A RU2010140375A RU2010140375A RU 2010140375 A RU2010140375 A RU 2010140375A RU 2010140375/04 A RU2010140375/04 A RU 2010140375/04A RU 2010140375 A RU2010140375 A RU 2010140375A RU 2010140375 A RU2010140375 A RU 2010140375A
- Authority
- RU
- Russia
- Prior art keywords
- hexaazatetracyclo
- hexanitro
- dodecane
- solution
- polymorphic composition
- Prior art date
Links
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 title claims abstract 29
- 238000004519 manufacturing process Methods 0.000 title 1
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract 8
- 238000002425 crystallisation Methods 0.000 claims abstract 4
- 230000008025 crystallization Effects 0.000 claims abstract 4
- 238000001704 evaporation Methods 0.000 claims abstract 4
- 238000000034 method Methods 0.000 claims abstract 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims abstract 4
- 238000005406 washing Methods 0.000 claims abstract 4
- 230000002378 acidificating effect Effects 0.000 claims abstract 3
- 230000018044 dehydration Effects 0.000 claims abstract 3
- 238000006297 dehydration reaction Methods 0.000 claims abstract 3
- 230000008020 evaporation Effects 0.000 claims abstract 3
- 239000012535 impurity Substances 0.000 claims abstract 3
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000000746 purification Methods 0.000 claims abstract 2
- 239000002253 acid Substances 0.000 claims 1
- 150000007513 acids Chemical class 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 238000010791 quenching Methods 0.000 abstract 1
- 230000000171 quenching effect Effects 0.000 abstract 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
1. Способ получения кристаллического 2,4,6,8,10,12-гексанитро-2,4,6,8,10,12-гексаазатетрацикло[5,5,03,11 ,05,9]додекана с заданным полиморфным составом путем кристаллизации из раствора 2,4,6,8,10,12-гексанитро-2,4,6,8,10,12-гексаазатетрацикло[5,5,03,11,05,9]додекана в ацетонитриле при внесении тетрахлорметана, отличающийся тем, что перед растворением 2,4,6,8,10,12-гексанитро-2,4,6,8,10,12-гексаазатетрацикло[5,5,03,11,05,9]додекана в ацетонитриле осуществляют его очистку путем отмывки раствора 2,4,6,8,10,12-гексанитро-2,4,6,8,10,12-гексаазатетрацикло[5,5,03,11,05,9]додекана в этилацетате от кислотных примесей, обезвоживания полученного раствора, упаривания с последующей обработкой этанолом. ! 2. Способ получения кристаллического 2,4,6,8,10,12-гексанитро-2,4,6,8,10,12-гексаазатетрацикло[5,5,03,11,05,9]додекана с заданным полиморфным составом путем кристаллизации из раствора предварительно очищенного 2,4,6,8,10,12-гексанитро-2,4,6,8,10,12-гексаазатетрацикло[5,5,03,11,05,9]додекана в 1,2-дихлорэтане в условиях резкого охлаждения, отличающийся тем, что очистку 2,4,6,8,10,12-гексанитро-2,4,6,8,10,12-гексаазатетрацикло[5,5,03,11,05,9]додекана осуществляют путем отмывки его раствора в этилацетате от кислотных примесей, обезвоживания полученного раствора, упаривания с последующей обработкой этанолом. 1. The method of obtaining crystalline 2,4,6,8,10,12-hexanitro-2,4,6,8,8,10,12-hexaazatetracyclo [5.5.03.13, 05.9] dodecane with a given polymorphic composition by crystallization from a solution of 2,4,6,8,10,12-hexanitro-2,4,6,8,8,12-hexaazatetracyclo [5.5,03,11,05,9] dodecane in acetonitrile with addition of carbon tetrachloride characterized in that before dissolving 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo [5.5,03,11,05,9] dodecane in acetonitrile it is purified by washing a solution of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo [5.5,03,11,05,9] dodecane in ethyl acetate from acidic when esey, dehydration of the resulting solution, evaporation followed by treatment with ethanol. ! 2. The method of obtaining crystalline 2,4,6,8,10,12-hexanitro-2,4,6,8,8,10,12-hexaazatetracyclo [5.5,03,11,05,9] dodecane with a given polymorphic composition by crystallization from a solution of pre-purified 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo [5.5,03,11,05,9] dodecane in 1, 2-dichloroethane under quenching, characterized in that the purification of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo [5.5,03,11,05 , 9] dodecane is carried out by washing its solution in ethyl acetate from acidic impurities, dehydrating the resulting solution, and evaporating, followed by By working with ethanol.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2010140375/04A RU2452739C9 (en) | 2010-10-01 | 2010-10-01 | Method of producing crystalline 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaaza-tetracyclo[5,5,0,03,11,05,9]dodecane having given polymorphous composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2010140375/04A RU2452739C9 (en) | 2010-10-01 | 2010-10-01 | Method of producing crystalline 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaaza-tetracyclo[5,5,0,03,11,05,9]dodecane having given polymorphous composition |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| RU2010140375A true RU2010140375A (en) | 2012-04-10 |
| RU2452739C1 RU2452739C1 (en) | 2012-06-10 |
| RU2452739C9 RU2452739C9 (en) | 2012-11-20 |
Family
ID=46031387
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| RU2010140375/04A RU2452739C9 (en) | 2010-10-01 | 2010-10-01 | Method of producing crystalline 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaaza-tetracyclo[5,5,0,03,11,05,9]dodecane having given polymorphous composition |
Country Status (1)
| Country | Link |
|---|---|
| RU (1) | RU2452739C9 (en) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5693794A (en) * | 1988-09-30 | 1997-12-02 | The United States Of America As Represented By The Secretary Of The Navy | Caged polynitramine compound |
-
2010
- 2010-10-01 RU RU2010140375/04A patent/RU2452739C9/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| RU2452739C1 (en) | 2012-06-10 |
| RU2452739C9 (en) | 2012-11-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2014521673A5 (en) | ||
| PT103661B (en) | MINOCYCINE PREPARATION PROCESS CRYSTALLINE | |
| EA201200716A1 (en) | METHOD FOR OBTAINING CRYSTALLINE FORMS A AND B IN ILAPRAZOL AND METHOD FOR TURNING THE INDICATED CRYSTALLINE FORMS | |
| FR2929960B1 (en) | PROCESS FOR PRODUCING CRYSTALLINE SILICON OF PHOTOVOLTAIC QUALITY BY ADDING DOPING IMPURITIES | |
| RU2015142819A (en) | SODIUM SALT (2S, 5R) -6-BENZYLOXY-7-OXO-1,6-DIAZA-Bicyclo [3.2.1] OCTAN-2-CARBONIC ACID AND ITS PRODUCTION | |
| RU2011106794A (en) | METHODS FOR EXTRACTION AND CLEANING OF THE INTERMEDIATE PRODUCT FOR PRODUCING SUCRALOSE | |
| AR078916A1 (en) | PROCEDURE FOR PURIFICATION OF PALIPERIDONA | |
| CN102875522B (en) | Method for purifying lactide | |
| MX2015016674A (en) | Compounds of '3-(5-sustituted oxy-2,4-dinitro-phenyl)-2-oxo-propi onic acid ester', process and applications thereof. | |
| AR081267A1 (en) | PROCEDURE FOR OBTAINING THE CRYSTAL FORM A OF FEBUXOSTAT | |
| RU2010140375A (en) | METHOD FOR PRODUCING CRYSTALLINE 2,4,6,8,10,12-HEXANITRO-2,4,6,8,10,12-HEXAAZATETRACYCLO [5,5,03,11,05,9] DODECAN WITH PRESENT POLYMORPHIC COMPOSITION (OPTIONS ) | |
| RU2019106531A (en) | Quinazoline derivative salt crystal | |
| CN102399200B (en) | Suspension crystallization method for preparing crystal form I of linezolid | |
| NO20090748L (en) | Procedure for cleaning montelukast | |
| CN103664805A (en) | Method for preparing acipimox | |
| JPWO2006028068A1 (en) | Method for purifying L-carnitine | |
| EA201291116A1 (en) | METHOD FOR PRODUCING METHANESULPHONATE SALTS OF RALFINAMIDE OR THEIR R-ENANTIOMERS | |
| RU2011143166A (en) | NEW CRYSTAL FORMS OF ADEFOVIR DIPIVOXIL AND METHODS OF ITS PRODUCTION | |
| FR2973799B1 (en) | PROCESS FOR OBTAINING A HEXANITROHEXAAZAISOWURTZITANE CRYSTAL CRYSTAL WITH ROUNDED MORPHOLOGY; CHARGE AND ENERGY MATERIAL CORRESPONDING | |
| RU2014112315A (en) | CRYSTAL FORM OF THIOTROPY BROMIDE | |
| RU2012122119A (en) | METHOD FOR PRODUCING A ROUTINE | |
| BR112014029361A2 (en) | Production method of terephthalic acid and its derivatives | |
| MX2014003509A (en) | Processes and intermediates for preparing a macrocyclic protease inhibitor of hcv. | |
| NZ598129A (en) | Process for the preparation of cathepsin s inhibitors | |
| EA201200241A1 (en) | NEW CRYSTAL FORM OF ORGANIC COMPOUNDS AND METHOD FOR ITS OBTAINING |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| TC4A | Altering the group of invention authors |
Effective date: 20120808 |
|
| TH4A | Reissue of patent specification | ||
| TK4A | Correction to the publication in the bulletin (patent) |
Free format text: AMENDMENT TO CHAPTER -FG4A- IN JOURNAL: 16-2012 FOR TAG: (54) |
|
| PD4A | Correction of name of patent owner | ||
| MM4A | The patent is invalid due to non-payment of fees |
Effective date: 20161002 |