Hydrochloric Acid → HCID 57523556, compound

Participants

Reaction Steps

To a solution of 6 (2.1 g, 8.3 mmol) in acetone (25 mL) was added 10% aqueous HCl solution (15 mL). The solution was cloudy. Thus, to the cloudy solution, was acetone dropwise (total 12 mL) until the solution was clear. The clear solution was stirred at room temperature for 5 h. The mixture was diluted with brine (250 mL). The aqueous mixture was extracted with methylene chloride/ether (1:2, 200 mL×3). The extract was washed with saturated aqueous bicarbonate solution (2×100 mL) and brine (100 mL×1), dried over MgSO4, and filtered. The filtrate was evaporated in vacuo to give 7 as a crystalline solid (1.7 g, 98%): 1H NMR (CDCl3) δ 2.75, 2.29, 2.04, 1.65 (each 2H, m), 1.32 (3H, s), 0.17 (9H, s); 13C NMR (CDCl3) δ 211.8, 110.8, 86.9, 39.2, 38.8, 32.9, 28.8, 0.4.

Provenance & Evidence