RU2013148717A - METHOD FOR PRODUCING POLYCYCLIC 3-ALKYL (PHENYL) PHOSPHOLAN-3-OXIDES - Google Patents
METHOD FOR PRODUCING POLYCYCLIC 3-ALKYL (PHENYL) PHOSPHOLAN-3-OXIDES Download PDFInfo
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- RU2013148717A RU2013148717A RU2013148717/04A RU2013148717A RU2013148717A RU 2013148717 A RU2013148717 A RU 2013148717A RU 2013148717/04 A RU2013148717/04 A RU 2013148717/04A RU 2013148717 A RU2013148717 A RU 2013148717A RU 2013148717 A RU2013148717 A RU 2013148717A
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Abstract
1. Способ получения полициклических фосфолан-3-оксидов формулы 1a-готличающийся тем, что каркасное непредельное соединение, выбранное из ряда бицикло[2.2.1]гептен-2, или экзо-трицикло[3.2.1.0]октен-6, или тетрацикло[4.3.0.0.0]нонен-8, или дициклопентадиен, взаимодействует с триэтилалюминием в присутствии катализатора CpZrCl, реакцию проводят при мольном соотношении реагентов CpZrCl: непредельное соединение: AlEt=0.01-0.1:1:1.05-1.1, в атмосфере аргона при температуре 15-25°C в течение 12 ч, затем в реакционную массу добавляют растворитель и при -10°C галогенид трехвалентного фосфора RPCl(где R=Ph, t-Bu, Me) в количестве 1:1 (моль/моль) по отношению к триэтилалюминию, реакционную массу перемешивают в атмосфере аргона при 15-25°C в течение 30 мин, после чего проводят окисление полученных фосфоланов 30% раствором HOв хлороформе в течение 1 ч.2. Способ получения по п.1, отличающийся тем, что в качестве растворителя используют толуол, бензол или гексан.1. A method of obtaining a polycyclic phospholan-3-oxide of the formula 1a-gotlichnyy in that the unsaturated framework compound selected from the series of bicyclo [2.2.1] hepten-2, or exo-tricyclo [3.2.1.0] octene-6, or tetracyclo [ 4.3.0.0.0] nonen-8, or dicyclopentadiene, interacts with triethylaluminum in the presence of a CpZrCl catalyst, the reaction is carried out at a molar ratio of CpZrCl reagents: unsaturated compound: AlEt = 0.01-0.1: 1: 1.05-1.1, in argon atmosphere at a temperature of 15 -25 ° C for 12 h, then the solvent and trivalent halide are added to the reaction mass at -10 ° C o phosphorus RPCl (where R = Ph, t-Bu, Me) in an amount of 1: 1 (mol / mol) in relation to triethylaluminum, the reaction mass is stirred in an argon atmosphere at 15-25 ° C for 30 minutes, after which oxidation of the obtained phospholans with a 30% HO solution in chloroform for 1 h. 2. The production method according to claim 1, characterized in that toluene, benzene or hexane are used as the solvent.
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RU2013148717/04A RU2551684C1 (en) | 2013-10-31 | 2013-10-31 | Method of producing polycyclic 3-alkyl(phenyl)phospholane-3-oxides |
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RU2013148717/04A RU2551684C1 (en) | 2013-10-31 | 2013-10-31 | Method of producing polycyclic 3-alkyl(phenyl)phospholane-3-oxides |
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RU2013148717A true RU2013148717A (en) | 2015-05-10 |
RU2551684C1 RU2551684C1 (en) | 2015-05-27 |
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RU2739242C1 (en) * | 2019-07-25 | 2020-12-22 | Федеральное государственное бюджетное учреждение науки Ордена Трудового Красного Знамени Институт нефтехимического синтеза им. А.В. Топчиева Российской академии наук (ИНХС РАН) | Method of producing high-density and high-energy rocket and aviation fuel component based on methyl-substituted 2,2'-bis (norbornanyl) (versions) |
RU2739190C1 (en) * | 2019-07-25 | 2020-12-21 | Федеральное государственное бюджетное учреждение науки Ордена Трудового Красного Знамени Институт нефтехимического синтеза им. А.В. Топчиева Российской академии наук (ИНХС РАН) | Method of producing high-density and high-energy rocket and aviation fuel based on 2-vinyl norbornane (versions) |
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RU2310660C1 (en) * | 2006-06-23 | 2007-11-20 | Институт нефтехимии и катализа РАН | Method for preparing 1-phenyl-2,5-dialkyl-3,4-fullero[60]phospholanes |
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