Ethanol, 2-(aminooxy)- → HCID 89443431, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of (81.3) (12 mg, 0.026 mmol) and 2-(aminooxy)ethanol (9.86 mg, 0.128 mmol) in MeOH (5 ml) was added 2 drops of HCl (2 N) by a 1-ml syringe to reach pH about 3 and the mixture was stirred in a sealed tube at 85° C. for 16 h. The mixture was evaporated to dryness and the residue was purified by preparative acid HPLC (gradient eluent NB from 20/80 to 95/5. mobile phase A: TFA/CH3CN 0.05%; mobile phase B: TFA/H2O 0.05%). The desired fractions were collected, evaporated by BUCHI under 30 mbar at 35° C. to remove CH3CN. The remained solution was lyophilized to afford title compound (11.5 mg, yield 85%).

Provenance & Evidence