HCID 86760776, compound → HCID 69224309, compound

Participants

Reaction Steps

In an autoclave, 38.1 g (158 mmol) of the crude product from Step 2.2 was suspended in 800 mL of ethanol and hydrogenated at 9 bar of hydrogen pressure for 2 hours using 3.8 g of Pd/C (10%). The catalyst was then filtered off through diatomaceous earth, to the filtrate was added 200 mL of 3M ethanolic hydrochloric acid, and the solution was concentrated to incipient crystallization in a rotary evaporator at 40° C. To complete the crystallization, the mixture was cooled in an ice bath, after which the solid was filtered off. The product was then washed with a small amount of ethyl acetate and dried at 40° C. under vacuum. This gave 19.5 g (41% of the theoretical) of a slightly pink-colored powder.

Provenance & Evidence