Hydrochloric Acid → HCID 14456755, compound

Participants

Reaction Steps

30 mg of the compound obtained in Example 4 was dissolved in 3 ml water. To this solution 3 ml ethyl acetate and 5 ml of diazomethane in ether were added, while cooling the solution with ice. After adding 83 μl of 1N hydrochloric acid, the resulting mixed solutio was stirred for 30 minutes, while cooling with ice. After 30 minutes of stirring, 8 ml of a solution of diazomethane in ether was added; the resulting mixed solution was stirred for 20 minutes, while cooling with ice. The reaction mixture, after dilution with water, was extracted with ethyl acetate. The organic layer was dried (MgSO4), then the solvent was evaporated under reduced pressure. The resulting residue was passed through a silica gel column and eluted with n-hexane-ethyl acetate (2:1), then the eluted fraction containing the desired product was collected and concentrated under reduced pressure to yield 13.5 mg of the subject compound in the form of a white crystal. Melting point: 182° to 184° C.

Provenance & Evidence