反応 #215404

反応方程式

sodium hydroxide

sodium cyanide

2-phenoxybenzyl chloride

butyl chloride

→

crude product

収率 92.8%

2-(2-Phenoxyphenyl)hexanenitrile

収率 92.8%

溶媒

dimethyl sulfoxide

water

反応条件

後処理

1. 1
   その他Reaction temperature
2. 2
   温度increases from 24° to 44° C
3. 3
   workup.STIRRINGAfter stirring for an additional 1/2 hour
4. 4
   その他reaction mixture
5. 5
   抽出extracted with hexane
6. 6
   洗浄The combined hexane extracts are washed with water
7. 7
   乾燥dried over MgSO4
8. 8
   その他Solvent is evaporated

実験手順

Into a three-necked 300 ml round-bottom flask are charged 7.4 g (0.15 mole) of sodium cyanide and 80 ml of dimethyl sulfoxide. To this slurry is added 30 g (0.13 mole) of 2-phenoxybenzyl chloride dropwise. Reaction temperature increases from 24° to 44° C. The reaction mixture is stirred for an additional 11/2 hours. To this reaction mixture is added 13.7 g (0.13 mole) of butyl chloride followed by dropwise addition of 34 g (0.4 mole) of 50% sodium hydroxide solution. After stirring for an additional 1/2 hour, reaction mixture is poured into 150 ml of water and extracted with hexane. The combined hexane extracts are washed with water and dried over MgSO4. Solvent is evaporated to give 32 g of crude product. Material can be further purified by vacuum distillation (bp 149-60/0.25 mm).

出典