Доклад № 19

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2020.m...@gmail.com

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Aug 27, 2020, 10:00:32 AM8/27/20
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Новый полиядерный силсесквиоксан меди и натрия с анизотропной формой молекулы: уточнение структуры по данным синхротронного РСА — Белякова Ольга Алексеевна, Астахов Г.С., Биляченко А.Н., Хрусталев В.Н.

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МИСС ФМ

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Aug 28, 2020, 3:59:22 AM8/28/20
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Новый полиядерный силсесквиоксан меди и натрия с анизотропной формой молекулы: уточнение структуры по данным синхротронного РСА — Белякова Ольга Алексеевна, Астахов Г.С., Биляченко А.Н., Хрусталев В.Н.


четверг, 27 августа 2020 г. в 21:00:32 UTC+7, МИСС ФМ:
Belyakova.pdf

yzubav

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Aug 28, 2020, 4:33:26 AM8/28/20
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А есть более подробная информация, как проводились каталитические испытания (слайд 5)?

пятница, 28 августа 2020 г. в 14:59:22 UTC+7, 2020.m...@gmail.com:

olbelyak

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Sep 1, 2020, 11:11:57 AM9/1/20
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Oxidation of Gaseous Alkanes.
 In a typical procedure, Cu(II) catalyst (1 µmol) was
combined with acetonitrile (up to 2.5 mL total reaction volume) in a stainless-steel
autoclave, followed by an addition of an acid promoter (optional, 20 µmol, typically
TFA), MeNO 2 (GC internal standard, 250 μL), and hydrogen peroxide (50% in H 2 O, 5
mmol). Then, the stainless-steel autoclave (total volume of 20.0 mL) was closed,
pressurized with a gaseous alkane substrate (2−3 atm), and kept under stirring at 50
°C (oil bath and magnetic stirrer) for 4−20 h. The autoclave was then cooled in an ice
bath and degassed. Samples of the reaction mixture were treated with PPh 3 and
analyzed by GC for quantification of products (internal standard method). Peaks were
attributed by comparing the obtained chromatograms with those of commercially
available samples of products. GC (Gas chromatography) analyses were carried out on
an Agilent Technologies 7820A series gas chromatograph (detector: FID; capillary
column: BP20/SGE; carrier gas: He).

Carboxylation of Gaseous Alkanes.
 In a typical procedure, Cu(II) catalyst (2 µmol),
H 2 O (2.0 mL), MeCN (4.0 mL), and K 2 S 2 O 8 (1.50 mmol) were introduced into a stainless
steel autoclave (total volume of 20.0 mL). Then, the autoclave was closed and first
flushed and pressurized with a gaseous alkane substrate (2-3 atm), followed by an
addition of CO (20 atm). The reaction mixture was stirred at 60 °C for 4 h (oil bath and
magnetic stirrer). After this period, the autoclave was cooled in an ice bath, degassed,
and opened. The reaction mixture was transferred to a glass flask. Et 2 O (9.0 mL) and
GC internal standard (cycloheptanone, 45 µL) were introduced. After stirring the
obtained mixture for 10 minutes, the aliquots were taken from an organic layer. These
were subjected to GC analysis for the quantification (internal standard method) of
carboxylic acids as principal products (ketones and alcohols are also formed in
different amounts as oxidation products). Peaks were attributed by comparing the
obtained chromatograms with those of commercially available samples of products. GC
(Gas chromatography) analyses were carried out on an Agilent Technologies 7820A
series gas chromatograph (detector: FID; capillary column: BP20/SGE; carrier gas:
He).

пятница, 28 августа 2020 г. в 15:33:26 UTC+7, yzubav:
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