反应 #1519134

反应方程式

2,3,4,5-tetrafluorobenzoyl chloride

Potassium ethyl malonate

MgCl2

→

Ethyl-(2′,3′,4′,5′-tetrafluorobenzoyl)-ethanoate

溶剂

acetonitrile

acetonitrile

反应条件

后处理

1. 1
   其他After removal of volatiles in vaccuo Toluene (30 ml)
2. 2
   workup.ADDITIONwas added
3. 3
   其他removed in vacuo
4. 4
   workup.ADDITIONthe addition of toluene (60 ml), HCl 1.5 M (40 ml)
5. 5
   workup.ADDITIONwas added cautiously
6. 6
   其他did not exceed 25° C
7. 7
   洗涤The organic fraction was washed with HCl 1.5 M (2×25 ml) and water (2×25 ml)
8. 8
   干燥dried over MgSO4

实验过程

Potassium ethyl malonate (3.66 g, 21.5 mmol), MgCl2 (2.44 g, 25.7 mmol) and TEA (2.05 g, 20.3 mmol) were mixed in acetonitrile (70 ml) at 10-15° C. for 2.5 hr. 2,3,4,5-tetrafluorobenzoyl chloride (2.00 g, 10.3 mmol) in acetonitrile (10 ml) was added at 0° C. over 15 min followed by a second addition of TEA (0.23 g, 2.3 mmol). After allowing to warm to RT, the mixture was stirred for 16 hr. After removal of volatiles in vaccuo Toluene (30 ml) was added and removed in vacuo. Following the addition of toluene (60 ml), HCl 1.5 M (40 ml) was added cautiously, ensuring the temperature did not exceed 25° C. The organic fraction was washed with HCl 1.5 M (2×25 ml) and water (2×25 ml), dried over MgSO4 and reduced to a light orange oil in vacuo ([M+1]+ 265, 98%).

来源