反应 #1183649

反应方程式

N-allyl-4-cyclohexene-1,2-dicarboximide

aminomethylphosphonic acid

→

4,5-epoxy-N-allylcyclohexane-1,2-dicarboximide

溶剂

hydrogen peroxide water

反应条件

后处理

1. 1
   其他In a 50 ml three-necked flask equipped with a reflux condenser
2. 2
   其他thermometer, stirrer, dropping
3. 3
   温度The mixture was heated
4. 4
   其他kept at 90° C.
5. 5
   温度After cooling with an ice bath
6. 6
   其他removing the excess hydrogen peroxide
7. 7
   萃取with 300 ml of saturated aqueous sodium thiosulfate, extraction
8. 8
   干燥The obtained ethyl acetate solution was dried overnight over anhydrous sodium sulfate
9. 9
   其他a rotary evaporator
10. 10
    其他to remove the ethyl acetate solvent
11. 11
    其他after which purification

实验过程

In a 50 ml three-necked flask equipped with a reflux condenser, thermometer, stirrer, dropping funnel and oil bath there were charged 100.0 g of N-allyl-4-cyclohexene-1,2-dicarboximide, 2.44 g of methyltrioctylammonium hydrogensulfate, 3.45 g of sodium tungstate dihydrate and 0.58 g of aminomethylphosphonic acid. The mixture was heated using an oil bath kept at 90° C., and after adding 80 ml of 30% hydrogen peroxide water dropwise over a period of 180 minutes through a dropping funnel, the mixture was aged for 4 hours. After cooling with an ice bath and removing the excess hydrogen peroxide with 300 ml of saturated aqueous sodium thiosulfate, extraction was performed twice with 200 ml of ethyl acetate. The obtained ethyl acetate solution was dried overnight over anhydrous sodium sulfate, and a rotary evaporator was used to remove the ethyl acetate solvent, after which purification was performed with a chromatography column packed with 25% hydrous silica gel to obtain 78.9 g of 4,5-epoxy-N-allylcyclohexane-1,2-dicarboximide.

来源