Dichloromethane cyclohexane → rac-4-Fluoro-2-methylbutane-1,2-diamine dihydrochloride

Participants

Reaction Steps

1.00 g (4.00 mmol) of rac-benzyl (2-cyano-4-fluorobutan-2-yl)carbamate from Example 73A were dissolved in 114 ml ethanol/glacial acetic acid (1/1), and 0.85 g of palladium on activated carbon (10%) were added. The reaction mixture was hydrogenated in an autoclave at 30-50 bar for 3 h. The reaction mixture was filtered through a fluted filter, rinsed with ethanol and then filtered once again through a Millipore filter. The filtrate was admixed with 10 ml of hydrogen chloride solution (2 N in diethyl ether) and then concentrated by evaporation. This gave 1.04 g of the target compound which was used in the subsequent stage without further purification.

Provenance & Evidence