Methanol → HCID 69417262, compound

Participants

Reaction Steps

In a round bottom flask fitted with a condenser, a suspension of the product from Step D (2.89 g; 7.60 mmol) in methanol (60 mL) was treated with concentrated H2SO4 (0.5 mL; cat.) and heated to reflux overnight. The reaction mixture was allowed to cool to room temperature, and the volatiles were removed in vacuo. The reaction was quenched with saturated aq. NaHCO3 solution and extracted with methylene chloride (5×). The combined extracts were washed with brine, dried (Na2SO4), filtered, and concentrated in vacuo. Trituration with methanol gave the desired product: m/e=392 (M+1).

Provenance & Evidence