Sodium Carbonate → HCID 10445156, compound

Participants

Reaction Steps

Ethyl chloroformate was added to 3-Amino-2,8-dimethyl-1-oxa-8-azaspiro[4.5]decane (1 g 5.4 mmol) in THF (20 ml). An additional 20 ml of THF were added and the reaction was stirred for 2 hours at room temperature. The THF solution was mixed with saturated sodium carbonate solution and the THF layer was separated, dried and evaporated to give a product which was purified by chromatography on silica gel and eluting with 5-10% ammoniated MeOH/CHCl3. The major fraction was converted to the fumaric acid salt in ether but a solid could not be obtained. The salt was neutralized with aqueous alkali and the base was extracted into methylene chloride. Concentration of the methylene chloride afforded the title carbamate compound as an oil.

Provenance & Evidence