反应详情

温度

-10 °C

A solution of 40 g of hydrogen chloride in 156 g of diethyl ether is added dropwise at room temperature to 96 g (0.84 mol) of 2,2-dimethyl-3-pentanone in 960 g of toluene. After cooling to −10° C., a solution of 95 g of n-butyl nitrite in 470 g of diethyl ether is added dropwise. The mixture is stirred at from −10° C. to 0° C. for 4 hours and then allowed to come to room temperature. After a total of 16 h, the reaction mixture is washed three times with 1 l of ice-water each time and then extracted twice with 1 l of 1M sodium hydroxide solution each time. The alkaline phase is separated off and neutralized with 20% strength sulfuric acid. The crude product is filtered off with suction and, after drying, recrystallized from n-hexane. 66 g (55%) of the title compound are obtained as a pale yellow powder of melting point 107-110° C.

1. customto come to room temperature
2. washAfter a total of 16 h, the reaction mixture is washed three times with 1 l of ice-water each time
3. extractionextracted twice with 1 l of 1M sodium hydroxide solution each time
4. customThe alkaline phase is separated off
5. filtrationThe crude product is filtered off with suction
6. customafter drying
7. customrecrystallized from n-hexane