反応 #94254

反応方程式

cyclohexyl isocyanate

1,3-dimethyl-3-hydroperoxybutyl alcohol

→

colorless solid

収率 39.0%

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

収率 39.0%

溶媒

ether

反応条件

後処理

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

実験手順

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.

出典