HRID229149
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
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
To a solution of (4-bromophenyl)[2-methyl-4-(methyloxy)phenyl]methanone (27) (1.12 g, 3.67 mmoL) in benzene (25 mL) was added AlCl3 (1.98 g, 14.85 mmol). The mixture was heated at 90° C. for 3 h. Upon cooling, water (25 mL) was added, and the mixture was extracted with Et2O. The organics were dried with MgSO4 and concentrated. The crude material was purified by chromatography on silica gel (EtOAc:hexanes) to yield 1.32 g (86%) of compound 28. 1H NMR (400 MHz, DMSO-d6): δ 2.26 (s, 3H), 6.63 (dd, J=2.4 Hz, 8.4 Hz, 1H), 6.72 (d, J=2.2 Hz, 1H), 7.18 (d, J=8.4 Hz, 1H), 7.55 (d, J=8.4 Hz, 2H), 7.70 (d, J=8.4 Hz, 2H), 10.10 (s, 1H).
WORKUP
后处理
- temperatureUpon cooling
- extractionthe mixture was extracted with Et2O
- dry with materialThe organics were dried with MgSO4
- concentrationconcentrated
- customThe crude material was purified by chromatography on silica gel (EtOAc:hexanes)