反応 #1869219

反応方程式

water

4,6-dichlororesorcinol

potassium carbonate

methyl bromoacetate

→

subtitle compound

収率 23.2%

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

収率 23.2%

溶媒

DMF

反応条件

後処理

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

実験手順

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.

出典