Bis(2-Methoxyethyl)amine → HCID 22064352, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 4-bromo-1-fluoro-2-nitrobenzene (0.44 g, 2mmol) and N,N-bis(2-methoxyethyl)amine (0.266 g, 2.4 mmol) in acetonitrile (10 mL) in a capped 20 mL vial was shaken at 80° C. overnight and concentrated. The concentrate was dissolved in methanol (10 mL), and treated with Raney nickel (50% water suspension, 0.40 g, 6.8 mmol). The vial was filled with excessive hydrogen, shaken at 50° C. for 1 hour, filtered, and concentrated. The concentrate was purified by preparative HPLC with acetonitrile/water containing 0.1% TFA to provide the desired product. MS (APCI(+)) m/z 304 (M+H)+.

Provenance & Evidence