Hydroxyamine hydrochloride → HCID 172983753, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of the product of Step A of Example 2 (0.12 g, 0.25 mmol), hydroxylamine hydrochloride (43.48 mg, 0.626 mmol) and TEA (0.087 mL, 0.626 mmol) in ethanol (1.2 mL) in a sealed tube in Ar was heated at 80° C. overnight. After removal of solvent, the residue was partitioned between EtOAc and brine, separated, dried over Na2SO4. Purification by CombiFlash (eluent: 8% methanol in DCM) gave the product as a white solid. 1H-NMR (400 MHz, CDCl3): δ 1.30-1.45 (m, 9H), 1.70-1.99 (m, 3H), 2.38 (br. s., 1H), 3.09 (d, J=9.3 Hz, 3H), 3.28-3.54 (m, 3H), 3.65-3.89 (m, 3H), 4.23 (d, J=5.1 Hz, 1H), 4.44-4.93 (m, 5H), 7.72 (br. s., 1H), 8.69 (s, 1H); LC/MS: C23H31F3N6O4: m/z 513 (M+H).

Provenance & Evidence