Dichloromethane → HCID 69113924, compound

Participants

Reaction Conditions

Reaction Steps

Amide compound 45 (2.7 g) was dissolved in CH2Cl2 (50 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 2 h. The excess HCl was degassed and the CH2Cl2 was removed. The residual sticky solid was dried under vacuum without further purification to yield the crude hydrochloride salt 53 (2.2 g, 94.8%). 1H NMR (DMSO-d6): 10.55 (b, 1H), 7.61 (d, J=8.0 Hz, 2H), 7.58 (d, J=8.4 Hz, 2H), 7.31 (overlapped d, J=8.4 Hz, 2H), 7.29 (d, J=8.4 Hz, 2H), 4.57 (m, 1H), 3.58 (s, 3H), 2.99-3.20 (m, 2H), 2.88 (t, J=7.6 Hz, 2H), 2.80 (s, 3H), 2.69 (s, 3H), 2.66 (t, J=7.6 Hz, 2H).

Provenance & Evidence