Diisopropylamine → HCID 131736048, compound

Temperature

125 °C

Diisopropylaminodiethylaminodisilane is synthesized in a pressurized reactor vessel by the reaction between disilane, diisopropylamine and diethylamine catalyzed by commercially available Ruthenium on carbon: A 0.3 L autoclave (reaction vessel) equipped with a mechanical stirrer, a thermocouple, a pressure gauge and a pressure transducer and 3 metering valves, as illustrated in FIG. 1, is charged with 6 g (0.003 mmol of ruthenium) of 5% weight ruthenium on carbon catalyst. The reactor is then heated under dynamic vacuum at 125° C. for 3 hr. activating the catalyst. After cooling to room temperature, the reactor is filled with helium at 1 atmosphere (“atm”) pressure, sealed and disconnected from the manifold. Inside a glove box, 20.7 g (0.205 mol) of diisopropylamine is added to the reactor. The reactor is taken out from the glove box and reconnected to the manifold and it is cooled to −130° C. in a liquid nitrogen bath. 30 g (0.453 mol) of disilane are transferred to the reactor through the manifold. The reactor is heated to about 150° C. The reactor contents is stirred at about 400 rpm for about 5 hr, pressure in the reactor increases about 160 psi. The reactor is cooled to RT. Volatiles are cryotrapped in a stainless steel lecture bottle (“SSLB”). The reaction vessel pressure drops to about 45 Torr. The reactor is put back in the glove box and is opened. 15.0 g (0.205 mol) of diethylamine are added to the mixture. They reactor is then heated to temperatures varying from about 30° C. to about 150° C. The reactor is stirred at about 400 rpm for about 2-24 hr. the pressure increases to about 160 psi. Volatiles are cryotrapped in a stainless steel lecture bottle (“SSLB”). The reaction vessel pressure drops to about 25-45 Torr. The diisopropylaminodiethylamino-disilane is recovered from the reaction vessel.

1. customA 0.3 L autoclave (reaction vessel)
2. customequipped with a mechanical stirrer
3. temperatureAfter cooling to room temperature
4. additionthe reactor is filled with helium at 1 atmosphere (“atm”) pressure
5. customsealed
6. temperatureis cooled to −130° C. in a liquid nitrogen bath
7. temperatureThe reactor is heated to about 150° C
8. temperaturepressure in the reactor increases about 160 psi
9. temperatureThe reactor is cooled to RT
10. temperatureThey reactor is then heated to temperatures
11. customvarying from about 30° C. to about 150° C
12. stirringThe reactor is stirred at about 400 rpm for about 2-24 hr
13. temperaturethe pressure increases to about 160 psi
14. customThe diisopropylaminodiethylamino-disilane is recovered from the reaction vessel

ORD record

ord-290406c0c9384a8a87bf6c9663f40343

Source dataset

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09382269B2