HRID1487202
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
- 130 °C
PROCEDURE
实验过程
To a solution of N-(8-bromo-2,3-dihydrobenzo[b][1,4]dioxin-5-yl)acetamide (5 g, 18.4 mmol) in toluene (50 mL) was added morpholine (1.9 g, 22 mmol), Pd2(dba)3 (1.68 g, 1.84 mmol), X-Phos (1.75 g, 3.68 mmol) and potassium tert-butoxide (4.1 g, 36.8 mmol) in a sealed tube. The mixture was heated at 130° C. for overnight. After cooled to room temperature, the mixture was filtered and the filtrate was evaporated to give a crude product, which was purified by silica gel column chromatography (petroleum ether/ethyl acetate 4/1) to afford the product N-(8-morpholino-2,3-dihydrobenzo[b][1,4]dioxin-5-yl)acetamide (2 g, yield 40%).
WORKUP
后处理
- temperatureAfter cooled to room temperature
- filtrationthe mixture was filtered
- customthe filtrate was evaporated
- customto give a crude product, which
- customwas purified by silica gel column chromatography (petroleum ether/ethyl acetate 4/1)