Dichloromethane → HCID 15982712, compound

Participants

Reaction Conditions

Reaction Steps

The acid compound 46 (0.9 g) was dissolved in CH2Cl2 (25 mL) and cooled to 0-5° C. Hydrogen chloride gas was bubbled through this solution for 20 min. The bubbling was discontinued and the reaction mixture was stirred at room temperature for 1 h. The excess HCl was degassed and the CH2Cl2 was removed. The residual solid was triturated with EtOAc (2×25 mL), decanted, and dried to yield the desired compound 50 as a white amorphous solid (0.64 g, 83%). 1H NMR (DMSO-d6): 12.2 (br, 1H), 7.62 (d, J=8.4 Hz, 2H), 7.56 (d, J=8.0 Hz, 2H), 7.31 (d, J=8.4 Hz, 2H), 7.29 (d, J=8.0 Hz, 2H), 4.58 (m, 1H), 3.02-3.08 (m, 2H), 2.85 (t, J=7.6 Hz, 2H), 2.81 (s, 3H), 2.71 (s, 3H), 2.57 (t, J=7.6 Hz, 2H).LCMS (m/e): Obsd. [MH]+ 341, Calcd. 340.4.

Provenance & Evidence