反应 #94254

反应方程式

cyclohexyl isocyanate

1,3-dimethyl-3-hydroperoxybutyl alcohol

→

colorless solid

收率 39.0%

1,3-Dimethyl-3-(N-cyclohexyl-carbamoylperoxy)butyl N-cyclohexylcarbamate

收率 39.0%

溶剂

ether

反应条件

后处理

1. 1
   workup.ADDITIONA mixture of 18.7 g
2. 2
   其他The reaction vessel was protected with a calcium chloride tube
3. 3
   过滤filtered
4. 4
   洗涤The filter cake was washed with an additional 30 ml of ether and air
5. 5
   其他dried

实验过程

A mixture of 18.7 g. (0.15 mole) of cyclohexyl isocyanate, 6.7 g. (0.05 mole) of 1,3-dimethyl-3-hydroperoxybutyl alcohol and 3 drops of triethylamine was stirred for 5 days at ambient temperature. The reaction vessel was protected with a calcium chloride tube to keep out moisture. Within 2 days, a solid began to appear, and after the 5 day stirring period the reaction mixture was stripped in vacuo. The residue was slurried in 100 ml of ether and filtered. The filter cake was washed with an additional 30 ml of ether and air dried. A total of 7.5 grams of a colorless solid was obtained.

来源