反応 #217497

反応方程式

2,3,4,5-tetrafluorobenzoyl chloride

Potassium ethyl malonate

MgCl2

→

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

溶媒

acetonitrile

acetonitrile

反応条件

後処理

1. 1
   その他After removal of volatiles in vacculo Toluene (30 ml)
2. 2
   workup.ADDITIONwas added
3. 3
   その他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
   その他did not exceed 25° C
7. 7
   洗浄The organic fraction was washed with HCl 1.5 M (2×25 ml) and water (2×25 ml)
8. 8
   乾燥dried over MgSO4

実験手順

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 vacculo 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%).

出典