Potassium Carbonate → 3-Methyl-6-phenyl-7-oxa-3-azabicyclo[4.1.0]heptane

Participants

Reaction Steps

A solution of 1-methyl-3-bromo-4-phenyl-4-piperidinol hydrobromide (4.10 g; 11.7 mmoles, described in Example 5) in water (5 ml) is cooled to 0°-5° C. Cold 10% aqueous sodium hydroxide solution (10 ml; 25 mmoles) is added dropwise with vigorous mechanical stirring, over a period of ten minutes. The solution is stirred for 30 min. and potassium carbonate is added to the solution at a temperature below 10° C. When the solution is saturated the solids are collected by filtration and crystallized from hexane at -70° C. to give the title compound, mp 44°-45° C. (R. E. Lyle and W. E. Krueger, supra, reported mp 43°-45° C.).

Provenance & Evidence