Hydrochloric Acid → HCID 135975028, compound

Participants

Reaction Steps

A solution of compound 6 (9.9 g) in EtOH (80 mL) was cooled to 0° C. with ice-water bath. Concentrated hydrochloric acid (37%, 40 mL) was added into the above solution slowly at 0° C. The ice-bath was removed and the mixture was stirred at rt until the reaction was complete as indicated by LCMS (ca. 5 h). A solution of NaHCO3 (40 g) in water (200 mL) was added slowly with stirring. The final mixture was extracted with EtOAc (˜200 mL), and the organic layer was washed with brine and dried over sodium sulfate. It was filtered, and the solvent was removed with rotavapor. The residua was dried under high vacuum to provide the title compound as pale yellow gum-like powder (6.5 g, 77.4%) and was used for next step without further purification. LCMS (ESI) m/z 562.39 (MH+), 259.26 (100); HPLC: tR=5.05 min.

Provenance & Evidence