反应详情

温度

10 °C

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.

1. additionAfter the addition
2. customto rise to 23° C
3. customthe benzene layer separated
4. washwashed with 30 ml
5. dry with materialwater, dried over anhydrous sodium sulfate
6. filtrationfiltered
7. custom(93% yield) resulted