Potassium Hydroxide → HCID 46199201, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of the product of Step E (0.009 g; 0.024 mmol) and AgNO3 (0.06 g; 0.14 mmol) in EtOH (0.2 ml) H2O (0.1 ml) was added at room temperature, followed by 10% KOH (0.1 ml). The resulting black suspension was stirred for 1 h at ˜50° C. and cooled to room temperature and filtered. The insoluble material was washed with H2O (2×0.2 ml). The combined filtrates were acidified to pH=1 with HCl and the product was taken up by extraction with EtOAc (2×5 ml). The organic phase was washed with brine, dried over anhydrous MgSO4, filtered and filtrate evaporated to dryness. The residue was purified by FCC (SiO2, CH2Cl2/acetic acid (AcOH) 98/2) to give the title compound (0.00012 g; 12.8%), as a creamy solid. 1H-NMR (CDCl3+CD3OD) 8.48 (s, 1H); 8.22 (m, 1H); 7.77 (m, 1H); 7.64-7.66 (m, 2H); 7.58 (s, 1H); 6.96 (d, 1H, J=6 Hz); 4.19 (m, 4H); 1.4-1.54 (m, 6H).

Provenance & Evidence