Hydrochloric Acid → HCID 9820749, compound

Participants

Reaction Steps

Diethyl 2,5-dimethyl-1-pyrrolin-5-yl)phosphonate prepared in step 1 above (4.87 g; 0.0208 mol) is placed in a 250 ml two-necked round-bottomed flask and diethyl phosphite (5.89 g; 0.043 mol) is added dropwise thereto. The reaction is stirred at room temperature for 5 days. The reaction mixture is treated with 0.1 M HCl solution to pH=1 and is then extracted with diethyl ether. The aqueous phase obtained is: treated by addition of NaHCO3 to pH=10. The amine is salted out by adding NaCl and a large excess of Na2CO3 with stirring, in the presence of diethyl ether. The aqueous phase is then extracted with diethyl ether, after which the organic phase is dried over anhydrous Na2SO4. After filtration and evaporation under vacuum, the title compound is obtained in the form of an orange oil (3.41 g, 44%).

Provenance & Evidence