HCID 9805655, compound → HCID 131722983, compound

Participants

Reaction Steps

To a suspension of the product from Example 170 (1.7 g, 3.5 mmol) in ethanol (35 mL) was added hydrochloric solution (37 wt % in water, 1.4 mL, 16.9 mmol) at 20° C. while stirring. The yellow slurry was heated to reflux for 1 h. A thick off-white slurry was gradually formed. The slurry was cooled to r.t., stirred for 20 h and filtered. The filter cake was washed with 40 mL of ethanol and dried at 45° C. vacuum oven for 24 h. The product was obtained as a pale yellow solid (1.8 g, 95% yield) with a HPLC purity of 99%; mp 202-208° C.; Anal. Calcd for C23H22ClN9O2.HCl: C, 52.28; H, 4.39; N, 23.86; Cl, 13.42. Found: C, 52.05; H, 4.41; N, 23.61; Cl, 13.09.

Provenance & Evidence