反应 #8463

反应方程式

4′-hydroxy-2′-methyl-acetophenone

1-bromo-3-chloropropane

potassium carbonate

→

title compound

2′-methyl-4′-chloropropoxyacetophenone

溶剂

acetone

反应条件

后处理

1. 1
   温度The reaction mixture was cooled to ambient temperature
2. 2
   其他partitioned between dichloromethane (200 mL) and water (200 mL)
3. 3
   洗涤The aqueous layer was washed twice with fresh portions of dichloromethane (200 mL) and brine
4. 4
   干燥dried over sodium sulfate
5. 5
   其他evaporated
6. 6
   workup.DISSOLUTIONThe residue was re-dissolved in dichloromethane (100 mL)
7. 7
   洗涤washed with 0.5 M sodium hydroxide (100 mL) and brine (100 mL)
8. 8
   干燥dried over magnesium sulfate
9. 9
   过滤filtered
10. 10
    其他evaporated

实验过程

A mixture of 4′-hydroxy-2′-methyl-acetophenone (10.5 g) and 1-bromo-3-chloropropane (7.6 mL) in acetone (70 mL) was treated with potassium carbonate (14.5 g). The mixture was stirred at 50° C. for approximately 18 hours. The reaction mixture was cooled to ambient temperature and partitioned between dichloromethane (200 mL) and water (200 mL). The aqueous layer was washed twice with fresh portions of dichloromethane (200 mL) and brine was used to break any emulsions. The organic fractions were combined, dried over sodium sulfate, and evaporated. The residue was re-dissolved in dichloromethane (100 mL) and washed with 0.5 M sodium hydroxide (100 mL) and brine (100 mL), dried over magnesium sulfate, filtered and evaporated to give the title compound which was used without further purification.

来源