HRID352062
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
- 80 °C
PROCEDURE
实验过程
Trifluoromethanesulfonic acid (4 ml) was ice-cooled, and 4-aminobutyric acid (1093 mg, 10.6 mmol) was added. Then, anisole (1 ml, 9.25 mmol) was added. The mixture was heated and stirred at 80° C. for 50 min. The mixture was cooled to room temperature and added dropwise to water (17 ml) under ice-cooling. The mixture was stirred under ice-cooling for 20 min and then at −10° C. for 30 min. The crystals were filtrated, washed with ice-cooled saturated brine, and dried under reduced pressure to give 4-amino-4′-methoxybutyrophenone trifluoromethanesulfonate (2.47 g, yield 78%).
WORKUP
后处理
- temperaturecooled
- temperatureThe mixture was heated
- temperatureThe mixture was cooled to room temperature
- temperaturecooling
- stirringThe mixture was stirred under ice-
- temperaturecooling for 20 min
- waitat −10° C. for 30 min
- filtrationThe crystals were filtrated
- washwashed with ice-
- temperaturecooled saturated brine
- customdried under reduced pressure