HRID1669328
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
- 0 °C
PROCEDURE
实验过程
4-Bromo-N-methoxy-3,N-dimethyl-benzamide (5.94 g, 23.05 mmol) was suspended in anhydrous tetrahydrofuran (200 mL), and cooled to 0° C. with stirring under nitrogen. 1-magnesium bromo-4-methyl-pentane (23 mL, 1.5M in tetrahydrofuran, 34.8 mmol) was slowly added to the reaction over 1 h. The reaction was allowed to warm slowly to room temperature and monitored by TLC. Upon complete consumption of starting material, the reaction was carefully neutralized with 1N hydrochloric acid, extracted with diethyl ether, washed, dried, and concentrated. The 1-(4-Bromo-3-methyl-phenyl)-5-methyl-hexan-1-one (5.2 g, 18.4 mmol) 80% yield, was used without further purification.
WORKUP
后处理
- temperatureto warm slowly to room temperature
- customUpon complete consumption of starting material
- extractionextracted with diethyl ether
- washwashed
- customdried
- concentrationconcentrated