Hydrochloric Acid → HCID 59415964, compound

Participants

Reaction Conditions

Reaction Steps

(Z)-Ethyl 3-(dimethylamino)-2-(2-fluoro-5-iodobenzoyl)acrylate (0.500 g, 1.28 mmol, Intermediate 24), N2,N2-dimethylpropane-1,2-diamine hydrochloride (0.177 g, 1.28 mmol), and potassium carbonate (0.194 g, 1.41 mmol) were combined in THF (10.0 mL). The reaction was heated at 60° C. for 2 hrs. After 2 h, DMF (5.0 mL) was added followed by potassium carbonate (0.530 g, 3.83 mmol). The reaction was heated at 90° C. for 6 h. The reaction mixture was cooled to 0° C. and 1N HCl was slowly added until pH was around 4. The resulting precipitate was filtered, washed with water and dried overnight to yield a light yellow solid (0.428 g).

Provenance & Evidence