Methanol → HCID 67337219, compound

Participants

Reaction Steps

To a solution of the intermediate from example 73 step C (Isomer B, 0.43 g, 0.92 mmol) in THF (30 mL) was added methanol (10 mL) followed by sodium hydroxide solution (2N, 2 mL, 4 mmol). The reaction was stirred at room temperature overnight. The reaction mixture was concentrated in vacuo to remove the organic solvents. The residue was acidified with 1N HCl until the pH was less than 2. The resulting solution was extracted with ethyl acetate (3×) dried over anhydrous Na2SO4, filtered and concentrated in vacuo to give the title compound as a white solid. This material was used in the next step without any further purification. 1H NMR (DMSO, 500 MHz): δ 7.86(d, J=8.5 Hz, 2H), 7.77(d, J=8.7 Hz, 2H), 7.67(s, 1H), 7.5(d, J=1.8 Hz, 2H), 7.14(d, J=8.3 Hz, 2H), 7.04(s, 1H), 6.98(d, J=8.9 Hz, 2H), 5.52(s, 2H), 3.77(s, 3H). LC-MS: 2.55 min; (M+H)=453.1.

Provenance & Evidence