Hydroxyamine hydrochloride → HCID 178431166, compound

Participants

Reaction Steps

2-Methyl-2-[[4-(1H-tetrazol-5-yl-methyl)phenoxy]-methyl]cyclohexanone (0.79 g, prepared in Example 3), hydroxylamine hydrochloride (0.22 g), sodium acetate (0.26 g) and ethanol (absolute, 20 ml) were combined and heated to reflux for 4 hours. The ethanol was removed in vacuo. The residue was partitioned between ethyl acetate and 10% HCl solution. The organic phase was washed with saturated aqueous NaCl solution, dried over MgSO4 and concentrated on the rotary evaporator. The product was triturated with dichloromethane-diethyl ether mixture to afford 0.47 g of white solid, mp 153°-156° C. Analytical HPLC showed the product was 97.7% pure.

Provenance & Evidence