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

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.

1. filtrationThe reaction mixture was filtered through
2. filtrationa fluted filter
3. washrinsed with ethanol
4. filtrationfiltered once again through a Millipore
5. filtrationfilter
6. concentrationconcentrated by evaporation
7. customThis gave 1.04 g of the target compound which was used in the subsequent stage without further purification

ORD record

ord-3e7f6ceac9ca4c5aacd70e5de1e04206

Source dataset

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09422285B2