Lithium Hydroxide → HCID 68492872, compound

Participants

Reaction Steps

To a stirred solution of compound 151 (35 mg, 0.064 mmol) in DCM (1 ml), was added DIEA (0.12 mmol, 19 μl) and nicotinoyl chloride hydrochloride (0.12 mmol, 17 mg).The solution was stirred at RT for 18 h, PS-trisamine was added then stirred at RT for 4 h. After filtration, the solution was washed with citric acid (10% aq) and NaHCO3 (sat, aq), the organic phase was dried over Na2SO4 and concentrated. The residue was dissolved in THF:MeOH (2:1, 1.5 ml). LiOH (1N aq, 3.2 mmol, 320 μl) was added. The solution was stirred at 60° C. for 24 h. Acetic acid was added and then concentrated. The residue was dissolved in MeOH and subjected to purification by HPLC, affording the title compound (19.5 mg, 0.03 mmol). Purity by HPLC>98%, M+H+633.1.

Provenance & Evidence