Hydrochloric Acid → HCID 23657703, compound

Participants

Reaction Steps

A solution of aluminum chloride (4.8 g, 11.43 mmol) in dry diethyl ether (70 mL) was added dropwise under Ar to a stirred suspension of lithium aluminum hydride (0.98 g, 25.78 mmol) in dry diethyl ether (100 mL). Pre-dried under high vacuum 82 (4.8 g, 11.43 mmol) was added in small portions. The reaction mixture was stirred at room temperature for 1 hour followed by careful addition of 2 M HCl (100 mL) and extraction with diethyl ether (2×100 mL). The ether solution was dried over CaCl2 and concentrated to provide 84 product as white crystals (3.84 g, 83%): mp 142-143° C. (diethyl ether). 1H NMR (DMSO-d6) δ7.60 (d, J=8.2 Hz, 2H), 7.47 (d, J=7.7 Hz, 2H), 7.24 (dd, J=8.2, 7.7 Hz, 2H), 6.80 (s, 2H), 4.52 (s, 2H). HPLC (method B) tR 10.67 min (100.00 area %). Anal. (C17H10Br2O3) C, H, Br.

Provenance & Evidence