反応 #63246

反応方程式

Sodium hydride

2-propyl-3,4-dichlorophenol

tetrahydrofuran

5-bromovaleronitrile

→

nitrile

4-(2-propyl-3,4-dichlorophenoxy)butane nitrile

溶媒

hexamethylphosphoramide

water

ethyl acetate

反応条件

後処理

1. 1
   workup.ADDITIONof a 60% dispersion in mineral oil) was added
2. 2
   温度The reaction mixture was cooled to room temperature
3. 3
   その他The solution was evaporated
4. 4
   workup.ADDITIONethyl acetate and water were added
5. 5
   その他The layers were separated
6. 6
   洗浄the ethyl acetate was washed several times with dilute hydrochlorid acid
7. 7
   ろ過The organic layer was filtered through sodium sulfate
8. 8
   その他evaporated

実験手順

To a solution of 37.1 g. of 2-propyl-3,4-dichlorophenol in 400 ml. of dry tetrahydrofuran and 25 ml. of hexamethylphosphoramide were added 32 ml. of 5-bromovaleronitrile. Sodium hydride (7.2 g. of a 60% dispersion in mineral oil) was added and the reaction was stirred for about three days at 65° C. The reaction mixture was cooled to room temperature and ethyl acetate and water were added. The solution was evaporated and ethyl acetate and water were added. The layers were separated and the ethyl acetate was washed several times with dilute hydrochlorid acid. The organic layer was filtered through sodium sulfate and evaporated to provide the desired nitrile intermediate. NMR.

出典