Methanesulfonic Acid → HCID 12082302, compound

Participants

Reaction Conditions

Reaction Steps

Methanesulfonic acid (11.6 g, 121 mmol) was added dropwise to a solution of the product from step B (10 g, 24.2 mmol) in CH2Cl2 (100 mL) over about 30 minutes. The reaction mixture was stirred for about 1 hour, then cooled to about 0° C., and then triethylamine (18.6 mL, 133.1 mmol) was added through an addition funnel. The mixture was allowed to warm to room temperature over about 1 hour, diluted with additional CH2Cl2 and washed with saturated aqueous NaCl, dried over Na2SO4, filtered and concentrated in vacuo to afford the product as a white solid (7.2 g). 1H-NMR (CDCl3) δ: 2.51-2.72 (m, 4H), 3.35 (m, 2H), 3.49 (m, 2H), 4.03 (m, 1H), 4.25 (m, 1H), 7.08 (d, 2H), 7.51 (t, 1H), 8.37 (d, 1H).

Provenance & Evidence