Hydrochloric Acid → HCID 19883286, compound

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Reaction Steps

The ester from Step 1 was hydrolyzed via the procedure of Step 7 Example 208. The solution was poured into 25 mL of water, conc. HCl added to adjust the solution to pH 1, and the water removed under vacuum. The crude product was stirred with 80 mL of 1:1 methanol/methylene chloride for 2 hours and the insoluble salts filtered off. The filtrate was evaporated to dryness to afford 0.444 g of the title compound as the hydrochloride salt., mp 224°-226° C., MS (DCl) M/Z 408 (M+H); NMR (TFA/AA) d 1.49 (m, 4H), 4.0-4.62 (m, 12H), 8.04 (d, 1H, J=13.5), 9.26 (s, 1H). Analysis calculated for C19H20ClF2N3O5 ·1.5 H2O: C, 48.47; H, 4.92; N, 8.92. Found: C, 48.23; H, 4.67; N, 8.61.

Provenance & Evidence