Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 86701829, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of N,O-dimethylhydroxylamine hydrochloride (650 mg, 0.67 mmol) in 2 mL of anhydrous THF under argon, 1M solution of LiN(TMS)2 in THF (1.32 mL, 1.32 mmol) at 0° C. were added dropwise. The mixture was stirred at 0° C. for 0.5 h then ethyl 1-methyl-8-oxo-1,4,5,6,7,8-hexahydrocyclohepta[c]pyrazole-3-carboxylate (50 mg, 0.22 mmol) in 5 mL of anhydrous THF at 0° C. were added dropwise. Ice bath was removed and the mixture was stirred at room temperature overnight. Water (20 mL) was added and the mixture was extracted with AcOEt (2×30 mL). The organic layer was dried over anhydrous Na2SO4 and the solvent evaporated to dryness. The crude solid was used without further purification. 52 mg (quantitative yield).

Provenance & Evidence