Acetic Acid → HCID 11753221, compound

Participants

Reaction Steps

Compound 17 was dissolved in 1 mL (1:1) trifluoroacetic acid (TFA) and CH2Cl2. The reaction stirred at room temperature for 2 h and concentrated under reduced pressure. The residue was dissolved in 4 mL CH2Cl2 and N-Methylmorpholine (NMM) (3.12 mmol). The reaction was stirred at 0° C. Acetic Acid (0.76 mmol) was added slowly to the reaction mixture and the mixture stirred at 0° C. for five min. Then 1-Hydroxylbenzotriazole hydrate (HOBt) (0.76 mmol) and 1-Ethyl-3-(3′-Dimethylaminopropyl)carbodiimide Hydrochloride (EDC.HCl) (0.76 mmol) were added sequentially. The reaction was stirred at room temperature for two h. CH2Cl2 was removed by reduced pressure and the residue dissolved in EtOAc. The organic layer was rinsed with a saturated NaHCO3 solution three times and once with Brine. The organic layer was dried with MgSO4, filtered and concentrated under reduced pressure. Compound 22 was purified by preparative HPLC.

Provenance & Evidence