Hydroxyammonium hydrochloride → HCID 178483759, compound

Participants

Reaction Conditions

Reaction Steps

The compound of Example 41(18.0 mg) and hydroxylammonium hydrochloride (20.0 mg) (Tokyo Kasei Ltd.) were dissolved in pyridine (0.5 ml) (Wako Pure Chemical Industries Ltd.) and the solution was stirred at 80° C. for 10 hours. The reaction mixture was diluted with dichloromethane and filtered through a glass filter. The solid obtained was dissolved in methanol and passed through a Mega Bond Elut SCX (Varian). The column was washed with methanol and the product was eluted with ammonia water (25%, Wako Pure Chemical Industries Ltd.)—methanol=5:95. The solvent was evaporated to dryness. The desired product was obtained as an orange solid. ESI−MS: m/z 350 (MH+); 1H-NMR (MeOH-d4): δ2.45 (6H, s), 2.74 (2H, t, J=6.3 Hz), 3.63 (2H, t, J=6.3 Hz), 6.81 (1H, dd, J=6.6 Hz, 2.3 Hz), 6.93 (1H, d, J=2.3 Hz), 7.77 (1H, d, J=5.3 Hz), 7.83 (1H, d, J=9.2 Hz), 8.42 (1H, d, J=5.3 Hz), 9.16 (1H, s).

Provenance & Evidence