Доклад № 19

[2020.m...@gmail.com]

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]

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:

[yzubav]

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]

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: