反応 #215043

反応方程式

mesityl oxide

pinanyl hydroperoxide

sulfuric acid

→

product

収率 56.9%

2-METHYL-2-PINANYLPEROXY-4-PENTANONE

収率 56.9%

反応条件

後処理

1. 1
   workup.ADDITIONA mixture of 11.8 g
2. 2
   洗浄of ether and washed with water, 5% sodium hydroxide solution and again with water to pH 8
3. 3
   workup.DISTILLATIONThe mixture was then subjected to steam distillation in the presence of sodium bicarbonate solution at 20 torr for 2 hours
4. 4
   その他to remove unreacted mesityl oxide and pinanyl hydroperoxide
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   その他the ether removed under reduced pressure
7. 7
   その他leaving 18.14 g

実験手順

A mixture of 11.8 g. (0.12 mole) of mesityl oxide and 25.40 g. (0.15 mole) of pinanyl hydroperoxide was stirred at 0° C. while 2.0 g. of 77% sulfuric acid solution was slowly added. The reaction mixture was allowed to warm slowly to 25° C. and stirred for a total of 16 hours. The organic layer was taken up in 30 ml. of ether and washed with water, 5% sodium hydroxide solution and again with water to pH 8. The mixture was then subjected to steam distillation in the presence of sodium bicarbonate solution at 20 torr for 2 hours to remove unreacted mesityl oxide and pinanyl hydroperoxide. The product was taken up in ether, dried over anhydrous magnesium sulfate and the ether removed under reduced pressure leaving 18.14 g. of product (56.9% yield).

出典