反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
An ethanolic solution of {4-[4-(3-Trifluoromethyl-phenyl)-1H-imidazol-2-yl]-cyclohexylmethyl}-carbamic acid benzyl ester (4.15 g, 0.0091 mol) and 10% Pd/Carbon (400 mg) was shaken overnight under 55 psi of hydrogen in a Paar apparatus. The mixture was filtered through celite and concentrated under reduced pressure to give a foam, which was triturated with EtOAc/Hexanes/MeOH to produce C-{4-[4-(3-trifluoromethyl-phenyl)-1H-imidazole-2-yl]-cyclohexyl}-methylamine as a filterable solid. 1H NMR (DMSO-d6): δ 0.93–1.05 (m, 2H), 1.30–1.4 (m, 2H), 1.42–1.55 (m, 2H), 1.85 (d, J=12.8 Hz, 2H), 1.99 (d, J=11.6 Hz, 2H), 2.4–2.5 (m, 1H), 2.56–2.66 (m, 1H), 7.43–7.48 (m, 1H), 7.50–7.55 (m, 1H), 7.63 (s, 1H), 7.99 (d, J=7.9 Hz, 1H), 8.02 (s, 1H). MS 324 (M+H)+
WORKUP
后处理
- filtrationThe mixture was filtered through celite and
- concentrationconcentrated under reduced pressure
- customto give a foam, which
- customwas triturated with EtOAc/Hexanes/MeOH