HCID 69805620, compound → HCID 9795553, compound

Participants

Reaction Conditions

Reaction Steps

305 g (0.85 mol) of benzyl 4-(2-(pyrimidin-2-ylcarbamoyl)vinyl)benzoate were hydrogenated in a 20 l Būchi autoclave in 8 l of 20% aqueous acetic acid in the presence of 25 g of 10% palladium/charcoal at, 40° C. under a hydrogen pressure of 2 bar. After 6 h and uptake of 65.76 l of hydrogen the reaction was finished. After standing overnight the mixture was warmed to 70° C. and the catalyst filtered off. The autoclave was washed with 3 l of 20% aqueous acetic acid at 70° C. The catalyst was washed with 1.5 l of 20% aqueous acetic acid at 70° C. The filtrate was evaporated under reduced pressure in a rotary evaporator and the residue was dissolved in 1 l of water with heating. Upon cooling to room temperature the product precipitated. The mixture was cooled to 0° C. to 5° C., the product was filtered off, washed with cold water and dried under reduced pressure at 50° C. Yield: 212 g (90.6%).

Provenance & Evidence