反应 #1869219

反应方程式

water

4,6-dichlororesorcinol

potassium carbonate

methyl bromoacetate

→

subtitle compound

收率 23.2%

Methyl (2,4-dichloro-5-hydroxyphenoxy)acetate

收率 23.2%

溶剂

DMF

反应条件

后处理

1. 1
   温度The resulting mixture was cooled
2. 2
   过滤Solid (bis-alkylated product) was filtered off
3. 3
   萃取was extracted with ether
4. 4
   其他the organics were dried
5. 5
   浓缩concentrated in vacuo
6. 6
   其他Purification by RPHPLC (Xterra, gradient 95-5%, ammonia (0.2% aq.) in acetonitrile)

实验过程

A mixture of 4,6-dichlororesorcinol (2 g), potassium carbonate (1.54 g) and methyl bromoacetate (1.71 g) in DMF (10 ml) was heated at 80° C. for 24 h. The resulting mixture was cooled and water (200 ml) added. Solid (bis-alkylated product) was filtered off, then the aqueous was acidified with aq. HCl, which was extracted with ether and the organics were dried and concentrated in vacuo. Purification by RPHPLC (Xterra, gradient 95-5%, ammonia (0.2% aq.) in acetonitrile) gave the subtitle compound (0.65 g) as a solid.

来源