反应详情

A solution of trans (4-cyanomethyl-cyclohexyl)-carbamic acid tert-butyl ester (0.71 g, 3.00 mmol) in DCM (15 mL) was treated with trifluoroacetic acid (2 mL) and the mixture was stirred at ambient temperature for 2.5 hours, then concentrated under vacuum. The residue was purified by column chromatography using Isolute SCX-2 cartridge (eluting with MeOH then 2M NH3 in MeOH). The relevant fractions were combined and concentrated under vacuum to afford 0.40 g (97%) of trans (4-amino-cyclohexyl)-acetonitrile that was used without further purification. 1H NMR (400 MHz, CDCl3) δ: 3.52-3.42 (m, 2H), 2.69-2.60 (m, 1H), 2.26 (d, 2H), 1.94-1.83 (m, 4H), 1.70-1.57 (m, 1H), 1.24-1.06 (m, 4H).

1. concentrationconcentrated under vacuum
2. customThe residue was purified by column chromatography
3. washeluting with MeOH
4. concentrationconcentrated under vacuum