反应详情

温度

60 °C

0.3 g of rhodium/activated carbon (5% Rh) was added to a solution of 1.90 g (7.8 mmol) of (S)-2-(cyanoacetyl-amino)-3-(1H-imidazol-4-yl)propionic acid, sodium salt (prepared according to Example 1) in 50 ml of ethanol/conc. ammonia solution (V:V=4:1). The mixture was hydrogenated at 110° C. and 45 bar for 1 h. This was followed by filtering off the catalyst and adjusting the filtrate to a pH of 8.2 with formic acid. After concentrating the solution under reduced pressure, the residue was suspended in 200 ml of ethanol and heated at 60° C. for 30 min. The product was filtered off, washed successively with ethanol, ethyl acetate and diethyl ether and finally dried.

1. customwas hydrogenated at 110° C.
2. filtrationby filtering off the catalyst
3. concentrationAfter concentrating the solution under reduced pressure
4. filtrationThe product was filtered off
5. washwashed successively with ethanol, ethyl acetate and diethyl ether
6. customfinally dried