反応 #1435727

反応方程式

hydrochloric acid

sodium hydride

diethyl carbonate

ethyl 2-chloro-6-fluorophenylacetate

→

diethyl (2-chloro-6-fluorophenyl)malonate

収率 87.7%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   workup.ADDITIONwere added dropwise
2. 2
   温度under heating
3. 3
   温度refluxed
4. 4
   温度under heating for 8 hours
5. 5
   温度The reaction mixture was cooled
6. 6
   抽出extracted with t-butyl methyl ether
7. 7
   洗浄The organic layer was washed with water
8. 8
   乾燥dried over sodium sulfate
9. 9
   濃縮concentrated

実験手順

Into a mixture of 7.2 g of sodium hydride (60% in oil), 17.0 g of diethyl carbonate and 150 ml of tetrahydrofuran, 26.0 g of ethyl 2-chloro-6-fluorophenylacetate were added dropwise under heating, and then refluxed under heating for 8 hours. The reaction mixture was cooled, poured into iced dil. hydrochloric acid and extracted with t-butyl methyl ether. The organic layer was washed with water, dried over sodium sulfate and concentrated. The residue was subjected to silica gel column chromatography to give 30.4 g of diethyl (2-chloro-6-fluorophenyl)malonate.

出典