反应详情

温度

0 °C

A suspension of lithium aluminum hydride (2.76 g, 72.6 mmol) in THF (225 mL) was cooled at 0° C. and a solution of trans-(4-azidomethyl-cyclohexylmethyl)-carbamic acid tert-butyl ester (15.0 g, 55.9 mmol) in THF (75 mL) was added over 1 hr. The reaction mixture was stirred at ambient temperature for 6 hr. The reaction was quenched with Na2SO4.10H2O, filtered through a pad of celite, and concentrated. The residue was purified by flash chromatography (silica gel, 50% MeOH in CHCl3) to give trans-(4-aminomethyl-cyclohexylmethyl)-carbamic acid tert-butyl ester (12.3 g, 91%) as a pale yellow oil.

1. customThe reaction was quenched with Na2SO4.10H2O
2. filtrationfiltered through a pad of celite
3. concentrationconcentrated
4. customThe residue was purified by flash chromatography (silica gel, 50% MeOH in CHCl3)