反応 #2045020

反応方程式

4-Nitro phenol

K2CO3

methyl chloroacetate

→

31

収率 72.5%

Methyl(4-Nitro phenoxy)acetate

収率 72.5%

溶媒

acetone

反応条件

後処理

1. 1
   温度refluxed for 12 hours
2. 2
   workup.DISTILLATIONAcetone was distilled off
3. 3
   workup.ADDITIONwater (1500 ml) added
4. 4
   ろ過Crude 31 was filtered
5. 5
   その他dried
6. 6
   その他recrystallised from a mixture of ethyl acetate:hexane (1:5)

実験手順

To a mixture of 4-Nitro phenol (100 g, 719 mmol) and anhydrous K2CO3 (400 g, 2.894 moles) in anhydrous acetone (950 ml) was added methyl chloroacetate (114 g, 1.050 moles) and refluxed for 12 hours. Acetone was distilled off and water (1500 ml) added. Crude 31 was filtered, dried and recrystallised from a mixture of ethyl acetate:hexane (1:5) to give pure 31 (110 g, 72.5%) as a white fluffy powder. M.p: 97-98.4° C.

出典