Dichloromethane → HCID 15982576, compound

Participants

Reaction Conditions

Reaction Steps

The acid compound 21 (0.8 g) was dissolved in CH2Cl2 (30 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 22 as a white amorphous solid (0.82 g, 85%). 1H NMR (CD3OD): 7.26 (overlapped d, J=8.8 Hz, 1H), 7.25 (overlapped d, J=8.8 Hz, 1H), 7.20 (d, J=8.8 Hz, 2H), 6.97 (overlapped d, J=8.4 Hz, 1H), 6.95 (overlapped d, J=8.4 Hz, 1H), 6.89 (overlapped d, J=8.4 Hz, 1H), 6.88 (overlapped d, J=8.4 Hz, 1H), 4.65 (m, 1H), 3.3-3.6 (m, 6H), 3.0-2.8 (m, 4H), 2.91 (t, J=7.6 Hz, 2H), 2.39 (t, J=7.6 Hz, 2H), 2.10(d, J=11.2 Hz, 3H). LCMS: Obsd. 455.0, Calcd. 454.52

Provenance & Evidence