Ethyl bromoacetate → HCID 6618951, compound

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Reaction Steps

A mixture of 6-hydroxy-spiro[2H-1-benzopyran-2,1'-cyclohexan]-4(3H)-one (prepared in Preparation 14) (0.878 g, 3.78 mmol), ethyl bromoacetate (0.69 g, 4.13 mmol), anhydrous potassium carbonate (0.78 g, 5.65 mmol) and dry N,N-dimethylformamide (DMF) (7.5 ml) is stirred at room temperature for 4 hours under nitrogen gas. DMF is removed by distillation under reduced pressure and the residue is extracted with diethyl ether. The ether layer is separated and washed successively with water, dilute sodium hydroxide and saturated brine, dried and distilled to remove ether. The residue is recrystallized from cyclohexane to obtain the title compound as a crystalline solid (1.11 g, yield 92.5%, m.p=72°-73° C.). ##STR10##

Provenance & Evidence