HCID 69028482, compound → HCID 17960605, compound

Participants

Reaction Steps

To a solution of the title compound of Step A (3.37 g, 75% pure) in ethanol (15 mL) was added palladium hydroxide (170 mg, 20 wt % on carbon). The flask was twice evacuated and flushed with nitrogen and then twice evacuated and flushed with hydrogen. The mixture was vigorously stirred under a balloon of hydrogen for 3 hours before being evacuated, exposed to air and filtered through a pad of Celite®. The solution was concentrated and filtered through a pad of silica gel, eluting with 1% then 5% then 10% methanol in dichloromethane, then 5% triethylamine, 10% methanol, 85% dichloromethane. The material eluting in triethylamine/methanol/dichloromethane was concentrated to give the title compound of Step B (1.5 g) as an off white solid.

Provenance & Evidence