反应详情

温度

-10 °C

A solution of 10.0 g (0.0768 mol) of decalin-1,3-dione in 50 ml of ethanol was magnetically stirred under nitrogen and cooled to -10° C. To the solution was added 7.77 g (0.0768 mol) of triethylamine followed by 15.14 g (0.0768 mol) of p-toluenesulfonylazide added all at once. The mixture was stirred for one hour at 0° C., and the solvent removed at reduced pressure at a temperature of less than 40° C. To the residue was added 200 ml of ether, and the ether removed to yield a yellow solid. This was recrystallized from ethanol to give 5.23 g of yellow crystals, mp 81°-83° C.

1. additionadded all at once
2. customthe solvent removed at reduced pressure at a temperature of less than 40° C
3. additionTo the residue was added 200 ml of ether
4. customthe ether removed
5. customto yield a yellow solid
6. customThis was recrystallized from ethanol