反应详情

温度

25 °C

A mixture of 2,2,3,3-tetramethylcyclopropane carboxylic acid (7.8g, 0.055M), potassium carbonate (3.8g, 0.0275M) water (40 mls), tetrabutylammonium bromide (1.5g, 10 mole %), alpha-cyano-3-phenoxybenzyl bromide (14.4g, 0.05 mole) and toluene (50 ml) was stirred at 25° C for 5 hours. The aqueous phase was separated and the toluene layer washed twice with 5% potassium carbonate solution and twice with water. The solution was filtered through a pad of silica-gel (3g) and evaporated to leave a pale-yellow oil (17.4g; purity = 92%). Recrystallisation of this material from hexane gave pure alpha-cyano-3-phenoxybenzyl 2,2,3,3-tetramethylcyclopropane carboxylate, melting point 50°-51° C.

1. customThe aqueous phase was separated
2. washthe toluene layer washed twice with 5% potassium carbonate solution and twice with water
3. filtrationThe solution was filtered through a pad of silica-gel (3g)
4. customevaporated
5. customto leave a pale-yellow oil (17.4g; purity = 92%)
6. customRecrystallisation of this material from hexane