反应 #409979

反应方程式

1-oxyl-4-hydroxy-2,2,6,6-tetramethylpiperidine

toluene

→

white solid

收率 30.0%

1-Benzyloxy-4-hydroxy-2,2,6,6-tetramethylpiperidine

收率 30.0%

溶剂

diethyl ether

反应条件

后处理

1. 1
   温度is heated in a pressure vessel for 53 hours
2. 2
   洗涤the resultant mixture is washed with 10 w/v % ascorbic acid (1×50 mL)
3. 3
   workup.DISTILLATIONdistilled water (2×50 mL)
4. 4
   干燥The organic phase is dried over anhydrous sodium sulfate
5. 5
   其他the volatiles are removed in vacuo
6. 6
   其他The residue is recrystallized from heptane

实验过程

A mixture of 2.58 g (0.015 mol) of 1-oxyl-4-hydroxy-2,2,6,6-tetramethylpiperidine and 27.64 g (0.30 mol) of toluene under a nitrogen atmosphere is heated in a pressure vessel for 53 hours. The reaction mixture is diluted with diethyl ether and the resultant mixture is washed with 10 w/v % ascorbic acid (1×50 mL) and distilled water (2×50 mL). The organic phase is dried over anhydrous sodium sulfate and the volatiles are removed in vacuo. The residue is recrystallized from heptane to give 0.59 g (30% yield) of a white solid melting at 86-87° C.

来源