Hydrochloric Acid → HCID 22901902, compound

Participants

Reaction Steps

A mixture of the product from Step E (158 g, 0.325 mol), THF (700 mL) and 2N HCl (180 mL) were stirred at room temperature for 20 hr. After evaporating the THF, the aqueous mixture was cooled to 0° C. and sodium bicarbonate (50 g) was carefully added followed by water (400 mL) and ethyl acetate (500 mL). The two layers were separated and the aqueous layer was extracted with ethyl acetate (250 mL). The combined organic extracts were washed with brine, dried (MgSO4) and evaporated to give a foam which was triturated with methylene chloride (200 mL) to give a solid (81.7 g, 75%): mp 144°-147° C. Recrystallization of this solid from methylene chloride gave an off-white solid: mp 163°-165° C.

Provenance & Evidence