Ethylenediamine → HCID 58747061, compound

Participants

Reaction Steps

To 340 mg (0.05 mmol) 131 resin 8 mL 1,2-ethylenediamine was added. The resin was agitated for 1 hr at ambient temperature then it was filtered off, washed twice with DMF. The filtrates were pooled and were evaporated to dryness. The remaining oily residue was dissolved in DMF and evaporated again in order to get rid of the amine traces. The crude material was dissolved in 5 mL aqueous 0.1% TFA solution and was purified on a preparative reverse phase HPLC column using acetonitrile gradient. The fractions containing the pure product were pooled, evaporated to dryness dissolved in 3 mL methanol and treated with 1 mL 4.0M HCl in dioxane. 133 was precipitated with ether as bis-HCl salt, filtered off and dried to yield 44.8 mg (88%). MS: 435.19 (M+H+).

Provenance & Evidence