Hydrochloric Acid → HCID 21309716, compound

Participants

Reaction Steps

The compound from step 40a (0.123 g, 0.44 mmol) was treated with saturated ethanolic HCl (5 mL) for 18 hr. The volatiles were removed in vacuo, and the dihydiochloride was washed with Et2O (3×20 mL), evaporated to dryness and recrystallized (EtOHIEt2O) to yield the title compound (0.074 g, 63%) as a white solid. mp 141-144° C. MS (DCI/NH3) m/e: 179 (M+H)+. 1H NMR (D2O, 300 MHz) δ: 8.33 (d, J=2.9 Hz, 1H), 7.89 (dd, J=9.0, 2.8 Hz, 1H), 7.64 (d J=8.8 Hz, 1H), 5.01-4.93 (m, 1H), 4.48 (d, J=4.4 Hz, 2H), 4.21-4.04 (m, 2H), 2.70 (q, J=8.5 Hz, 2H), 2.62 (s, 3H). Anal. calc. for C10H16Cl2N2O.1.0H2O: C, 44.62; H, 6.74; N, 10.41. Found: C, 44.55; H, 7.02; N, 10.50. [α]D24 -7.89 ° (c=0.19 in MeOH).

Provenance & Evidence