Diisopropyl Ether → HCID 58124898, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 100 mg of 12j and 150 mg of anhydrous sodium acetate in 4 ml of acetic anhydride was heated at 100-105° C. for 2 h. The mixture was cooled and diluted with 10 ml of water and stirred at ambient temperature for 1 hr in order to decompose excess anhydride. The reaction mixture was neutralized by addition of cold conc. aq. NH4OH and then extracted with ethyl acetate. The extract was washed twice with water, dried, concentrated and the residue was purified by chromatography over silica gel, using a gradient of heptane/ethyl acetate. The purified product thus isolated was treated with diisopropyl ether, to give 65 mg of crystalline 12k; Mp 173-175° C.; Rf 0.45 (heptane/ethyl acetate 1/1). MS-ESI: [M+1] 484.96, 586.98.

Provenance & Evidence