HRID2037494
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
To a solution of [1-(4-bromo-phenyl)-ethyl]-[2-(2-isopropyl-[1,3]dioxolan-2-yl)-ethyl]-amine (14.5 g, 0.042 mol) in MeOH (70 mol) was added HCl (36%, 70 mol). The mixture was stirred at 65° C. till the reaction was over. The mixture was cooled to 0° C. The pH of the mixture was adjusted to 7. The mixture was condensed, and the residue was extracted with EtOAc. The organic phase was dried over Na2SO4, and concentrated to give the crude 1-[1-(4-bromo-phenyl)-ethylamino]-4-methyl-pentan-3-one (10.3 g, crude), which was used for the next step without further purification. 1H NMR (CDCl3): 1.08 (m, 6H), 1.35 (m, 3H), 2.51-2.70 (m, 6H), 3.72 (m, 1H), 7.19 (m, 2H), 7.42 (m, 2H).
WORKUP
后处理
- temperatureThe mixture was cooled to 0° C
- customcondensed
- extractionthe residue was extracted with EtOAc
- dry with materialThe organic phase was dried over Na2SO4
- concentrationconcentrated