Lithium Hydroxide → HCID 67215068, compound

Participants

Reaction Steps

A solution of LiOH (800 μL of a 2 M solution in H2O) was added to a solution of 68G (50 mg, 0.16 mmol) in 4 mL of a 3:1 mixture MeOH/H2O. After 1 hour, the reaction was complete as shown by TLC. The reaction mixture was then concentrated and the residue was dissolved in water and HCl 10% was then added. As no product precipitated, the aqueous solution was extracted 3 times with AcOEt. The combined organic layers were washed with brine, dried over MgSO4 and concentrated. A white foamy solid was obtained and used in the next step without further purification (47 mg, quantitative). NMR 1H (ppm, DMSO-d6): 7.86 (s, 1H), 7.61-7.60 (m, 3H), 7.57 (s, 1H), 7.46-7.33 (m, 3H), 6.16 (br, s, 1H), 3.72 (s, 2H), 3.70 (s, 3H), 3.46-3.39 (m, 2H), 1.64 (sext., J3=7.43 Hz, 2H), 0.98 (t., J3=7.50 Hz, 3H).

Provenance & Evidence