Synthetic Route of 4461-39-6, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 4461-39-6, name is N-(2-Hydroxyethyl)-1,3-propanediamine. A new synthetic method of this compound is introduced below.
A stirred 20 L glass reactor was charged with sulfolane (14.2 kg) and 2-(3- aminopropylamino)ethanol (1.29 kg, 10.9 mol) at 90C. The solution was sparged with nitrogen through a Hasteloy C dip-leg, then anhydrous hydrogen bromide (total 1.77 kg, 21.9 mol) was slowly admitted below the liquid surface. The temperature during addition was allowed to rise to 119C during addition, the solution was stirred for 15 minutes and was then allowed to stand at 110C under nitrogen purge overnight. The solution temperature was raised to 120C and, using a Masterflex pump and 1/8 inch diameterTefion tubing, phosphorus tribromide (1.034 kg, 3.82 mol) was added over one hour. The tubing was rinsed into the reactor with more sulfolane (0.60 kg). While stirring rapidly at 1200C, nitrogen was bubbled through the dip-leg for one hour to remove excess HBr.[00039] To a stirred 30 L reactor under nitrogen containing acetone (16.8 kg), one-half of the hot sulfolane solution was transferred using a Vi inch diameter PTFE tube. The acetone slurry was stirred 15 minutes and then the reactor was drained into a polyethylene bench-top vacuum filtration funnel that was kept under nitrogen using a metal cover. The 30 L reactor was again charged with acetone (16.9 kg), purged with nitrogen, and the remaining hot sulfolane solution was transferred from the 20 L reactor. After stirring, the slurry was discharged and filtered into the same bench-top funnel. The 30 L reactor was charged with more acetone (6.8 kg), purged with nitrogen and heated to 50C. The hot acetone was carefully drained into the funnel and, under nitrogen, the combined solids were washed and filtered. This hot acetone wash was repeated in order to effectively remove sulfolane. The
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4461-39-6, its application will become more common.
Reference:
Patent; ALBEMARLE CORPORATION; WO2007/53730; (2007); A1;,
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