Ethylenediamine → HCID 17854996, compound

Temperature

25 °C

In a 500 mL, 3-necked round-bottomed flask were taken 5.31 grams of 1,2-ethylenediamine and 32.48 g of anhydrous potassium carbonate, and 300 mL of chloroform. To this suspension was added 30 g of 4-vinylbenzyl chloride. The resulting reaction mixture was stirred at 25° C. for 18 hr. Subsequently the reaction mixture was filtered. The solvent was moved under reduced pressure. To the residue was added 300 mL of deionized water followed by 37% aqueous HCl until the pH of the solution was 2.0. The resulting aqueous solution was extracted with tert-butyl methyl ether (2×250 mL). The aqueous layer was collected and was treated with 40% (w/w) NaOH until the pH of the solution was 11.4. The resulting aqueous solution was extracted with tert-butyl methyl ether (2×250 mL). The organic layers were combined and dried over anhydrous sodium sulfate. After filtration, the solvent was removed under reduced pressure yielding 3 g of the product as a light yellow oil.

1. customThe resulting reaction mixture
2. filtrationSubsequently the reaction mixture was filtered
3. additionTo the residue was added 300 mL of deionized water
4. extractionThe resulting aqueous solution was extracted with tert-butyl methyl ether (2×250 mL)
5. customThe aqueous layer was collected
6. additionwas treated with 40% (w/w) NaOH until the pH of the solution
7. extractionThe resulting aqueous solution was extracted with tert-butyl methyl ether (2×250 mL)
8. dry with materialdried over anhydrous sodium sulfate
9. filtrationAfter filtration
10. customthe solvent was removed under reduced pressure

ORD record

ord-c99bb742d82c4fa084501594d7827062

Source dataset

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08986669B2