反応 #459149

反応方程式

4-t-butylazo-4-cyanovaleryl chloride

sodium hydroxide

hydrogen peroxide

water

→

Di[4-t-Butylazo-4-cyanovaleryl] peroxide

収率 93.0%

溶媒

benzene

benzene

反応条件

後処理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   その他to rise to 23° C
3. 3
   その他the benzene layer separated
4. 4
   洗浄washed with 30 ml
5. 5
   乾燥water, dried over anhydrous sodium sulfate
6. 6
   ろ過filtered
7. 7
   その他(93% yield) resulted

実験手順

To a solution of 0.48 g. (.012 m) of sodium hydroxide and 0.40 g. (.006 m) of 50% hydrogen peroxide in 10 ml. water at 10° C was added a solution of 2.7 g. (.0118 m) of 4-t-butylazo-4-cyanovaleryl chloride in 10 ml. benzene over 5 minutes. After the addition was complete, the reaction was stirred an additional 1/2 hour at 10° C and 15 minutes more allowing the temperature to rise to 23° C. Another 10 ml. benzene was added, the benzene layer separated, washed with 30 ml. 10% NaHCO3 solution, 15 ml. water, dried over anhydrous sodium sulfate, filtered and the benzene stripped off. A white crystalline solid weighing 2.3 g. (93% yield) resulted.

出典