RU2220969C2 - Method for preparing 1-ethyl-3-alkyl(phenyl)-6,7- -fullereno[60]cyclohepta-2-ox-1-alanes - Google Patents

Method for preparing 1-ethyl-3-alkyl(phenyl)-6,7- -fullereno[60]cyclohepta-2-ox-1-alanes Download PDF

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RU2220969C2
RU2220969C2 RU2002100654/04A RU2002100654A RU2220969C2 RU 2220969 C2 RU2220969 C2 RU 2220969C2 RU 2002100654/04 A RU2002100654/04 A RU 2002100654/04A RU 2002100654 A RU2002100654 A RU 2002100654A RU 2220969 C2 RU2220969 C2 RU 2220969C2
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preparing
catalyst
room temperature
argon atmosphere
fullereno
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RU2002100654A (en
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У.М. Джемилев
А.Г. Ибрагимов
Л.О. Хафизова
А.Л. Борисова
Л.М. Халилов
Ю.В. Томилов
О.М. Нефедов
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ГУ Институт нефтехимии и катализа АН РБ и УНЦ РАН
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Abstract

FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to methods for preparing new organoaluminum compounds that can be used in organic and metalloorganic synthesis. Invention describes method for preparing 1-ethyl-3-alkyl(phenyl)-6,7-fullereno[60]cyclohepta-2- ox-1-alanes of the formula:
Figure 00000002
wherein R is n-C3H7, n-C5H11,; Ph; n = 1-3; C60 is allotropic modification of carbon by interaction of fullerene[60] with triethylaluminium (EtAl3) excess in the presence of zirconacene dichloride (Cp2ZrCl2) as a catalyst in argon atmosphere at room temperature for 24 h in toluene medium followed by addition at temperature 15 C of cuprous chloride CuCl as a catalyst and aldehyde RCHO wherein R has above indicated values followed by stirring reaction mass in argon atmosphere at room temperature for 6-10 h. EFFECT: improved preparing method. 2 cl, 1 tbl, 1 ex

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Текст описания в факсимильном виде (см. графическую часть)а Description text in facsimile form (see graphic part) a

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Способ получения 1-этил-3-алкил(фенил)-6,7-фуллерено[60]-циклогепта-2-окс-1-аланов общей формулы (I)The method of obtaining 1-ethyl-3-alkyl (phenyl) -6,7-fullereno [60] -cyclohepta-2-ox-1-alans of the general formula (I)
Figure 00000009
Figure 00000009
где R = н-C3H7, н-C5H11, Ph;where R = n-C 3 H 7 , n-C 5 H 11 , Ph; n = 1÷3, С60 - аллотропная модификация углерода,n = 1 ÷ 3, C 60 - allotropic modification of carbon, отличающийся тем, что фуллерен [60] взаимодействует с избытком триэтилалюминия (АlЕt3), взятыми в мольном соотношении C60:AlEt3=1:(30÷50), в присутствии катализатора цирконацендихлорида (Ср2ZrСl2) в количестве 0,5-1,5 мол.% по отношению к триэтилалюминию в атмосфере аргона при комнатной температуре в присутствии толуола в качестве растворителя, в течение 24 ч, с последующим добавлением при температуре -15°С катализатора однохлористой меди (CuCl) в количестве 0,5-1,5 мол.% по отношению к триэтилалюминию и альдегида формулы RCHO, где R = н-C5H7, н-С5Н11, Рh, в эквимольном по отношению к триэтилалюминию количестве, после чего реакционную массу перемешивают при комнатной температуре в атмосфере аргона в течение 6-10 ч.characterized in that the fullerene [60] is reacted with an excess of triethyl aluminum (AlEt 3) taken in a molar ratio of C 60: AlEt3 = 1: (30 ÷ 50), in the presence of a catalyst tsirkonatsendihlorida (Cp 2 ZrSl 2) in an amount of 0.5- 1.5 mol.% With respect to triethylaluminum in an argon atmosphere at room temperature in the presence of toluene as a solvent, for 24 hours, followed by the addition of a catalyst of copper monochloride (CuCl) in an amount of 0.5-1 at a temperature of -15 ° C 5 mol.% with respect to the triethyl aluminum and an aldehyde of formula RCHO, where R = n-C 5 H 7, n-C 5 H 11, Ph, in equimolar SG with respect to an amount of triethylaluminum, and the reaction was stirred at room temperature under an argon atmosphere for 6-10 h.
RU2002100654/04A 2002-01-04 2002-01-04 Method for preparing 1-ethyl-3-alkyl(phenyl)-6,7- -fullereno[60]cyclohepta-2-ox-1-alanes RU2220969C2 (en)

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