反应详情

A suspension of 13 g (65 mmoles) of crude (11) in 75 mL 1N hydrochloric acid was warmed on a steam bath until a clear solution was obtained. After 1 h at room temperature crystals were noted. The mixture was chilled overnight and the crystals were filtered and dried to provide 13.86 g of title compound (12), mp 162° C. Anal. Calcd. for C9H18N3O2Cl: C, 45.86; H, 7.70; N, 17.83; Cl, 15.04. Found: C, 45.90; H, 7.64; N, 17.88; Cl, 14.79.

1. temperaturewas warmed on a steam bath until a clear solution
2. customwas obtained
3. temperatureThe mixture was chilled overnight
4. filtrationthe crystals were filtered
5. customdried