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
Palladium on carbon (10 wt %, 67.5 mg, 0.063 mmol) was added to a solution of morpholin-4-yl(5-nitrobiphenyl-3-yl)methanone (198 mg, 0.634 mmol) in ethyl acetate (5.7 mL) and acetic acid (0.57 mL). The mixture was fitted with a hydrogen balloon and stirred for 3 hours at room temperature. Dichloromethane was added, and the mixture was filtered through CELITE, rinsed with dichloromethane rinse and washed with saturated aqueous NaHCO3 (30 mL). The organic extracts were dried over sodium sulfate, filtered, and concentrated in vacuo to provide (5-aminobiphenyl-3-yl)(morpholin-4-yl)methanone as a white solid which was used without further purification. 1H NMR (400 MHz, CDCl3) δ 7.61-7.51 (m, 2H), 7.44 (t, J=7.4 Hz, 2H), 7.37 (dd, J=8.4, 6.2 Hz, 1H), 6.97 (s, 1H), 6.96-6.91 (m, 1H), 6.75-6.63 (m, 1H), 3.89 (s, 2H), 3.85-3.37 (m, 8H).
WORKUP
后处理
- filtrationthe mixture was filtered through CELITE
- washrinsed with dichloromethane
- washrinse
- washwashed with saturated aqueous NaHCO3 (30 mL)
- dry with materialThe organic extracts were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo