反応 #1172511

反応方程式

potassium

4-hydroxyacetophenone

methyl 2-chloropropanoate

→

methyl 2-(4-acetylphenoxy)propanoate

収率 80.4%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   ろ過The reaction is filtered
2. 2
   その他to remove KCl
3. 3
   濃縮the filtrate is concentrated under reduced pressure
4. 4
   その他to remove DMF
5. 5
   workup.DISSOLUTIONThe product is dissolved in ethyl acetate (300 mL)
6. 6
   抽出extracted with 2N NaOH (2×100 mL) and water (100 mL)
7. 7
   その他The organic phase is dried
8. 8
   濃縮concentrated

実験手順

To a solution of the potassium salt of 4-hydroxyacetophenone (25.0 g, 0.14 mol) in dimethylformamide (DMF) (100 mL) is added methyl 2-chloropropanoate (24.5 g, 0.20 mol) over 30 minutes and stirred at 85-90° C. for 3 hours under nitrogen. The reaction is filtered to remove KCl and the filtrate is concentrated under reduced pressure to remove DMF and the product analyzed by GLC. The product is dissolved in ethyl acetate (300 mL) and extracted with 2N NaOH (2×100 mL) and water (100 mL). The organic phase is dried and concentrated to give pure methyl 2-(4-acetylphenoxy)propanoate (25 g) (yield 64%).

出典