ChemicalBook CAS DataBase List 1-Hexene

1-Hexene synthesis

13synthesis methods

Product Name:1-Hexene
CAS Number:592-41-6
Molecular formula:C6H12
Molecular Weight:84.16

74-85-1
115 suppliers
$79.00/11l

592-41-6
273 suppliers
$10.00/5g

111-66-0 Synthesis

111-66-0
177 suppliers
$10.00/10ml

Yield:592-41-6 99.45% ，111-66-0 95.8%

Reaction Conditions:

Stage #1: ethenewith chromium(III) acetylacetonate;C₂₃H₄₉N₃P₂ in n-heptane;toluene at 5 - 130; under 22502.3 Torr; for 1 h;Inert atmosphere;Schlenk technique;
Stage #2: in n-heptane;toluene; under 150.015 Torr; for 0.166667 h;Inert atmosphere;Reagent/catalyst;

Steps:

2 Catalyst Composition Preparation and Oligomerization of Ethylene

The reactor, equipped with dip tube, thermowell, mechanical paddle stirrer, cooling coil, control units for temperature, pressure and stirrer speed (all hooked up to a data acquisition system) was prepared for the catalytic run by heating to 130° C. in under vacuum for 4 hours and cooled down by venting with dry nitrogen stream to 30° C. An isobaric ethylene supply was maintained by gas dosing control unit connected to data acquisition system. Ethylene consumption was monitored via pressure loss in the feeding cylinder over time by means of a computerized data acquisition system. Suitable amounts of the stock toluene solutions of the ligands and Cr(III)acetylacetonate as chromium precursor, at a ligand to Cr ratio of 1.20, were measured and charged to a Schlenk tube under inert atmosphere. A volume of 30 mL anhydrous n-heptane was introduced in stainless steel pressure reactor and warmed up to desired reaction temperature. After temperature of the reactor become stable, reactor was pressurized to 30 bar of ethylene and left for 30 min with continuous mechanical stirring. After that time, pressure was reduced to 0.2 bar and appropriate amount of 0.3M stock solution of MMAO-3A in anhydrous n-heptane was introduced in the reactor through the charging port, providing Al to Cr ratio of 300. Stirring was continued for 10 min. Following that, mixture of Cr and ligand solutions was introduced into the reactor through the charging port. Immediately after introduction of the catalyst in the reactor, pressure was increased to 30 bar. Standard reaction conditions are: pressure of ethylene of 30 bar, T=45° C., stirrer speed of 450 RPM. After 1 hour catalytic run, ethylene supply was cut and reactor temperature lowered to 5° C. Ethylene from the reactor was vented to the pressure of 0.2 bar. The reaction was quenched with 0.3M HCl/iso-Propanol mixture. It should be noted that it is also possible to quench the reaction with different agents, such as Decan-1-ol, 2-EHA, 20% wt. NaOH in water. Liquid products were analyzed using gas chromatography with a known amount of toluene as internal standard. Any insoluble by-products, i.e., waxes, polyethylene, were filtered, dried, and weighed. Table 1 shows the results of ligand

References:

US2022/1368,2022,A1 Location in patent:Paragraph 0054-0056

74-85-1
115 suppliers
$79.00/11l

592-41-6
273 suppliers
$10.00/5g

References

111-14-8 Synthesis