反应详情

温度

0 °C

58.5 g (0.79 mol) of tert-butanol are added with stirring at 0° C. under argon to 100 g (0.79 mol) of oxalyl chloride in 1.3 l of THF. After stirring at 0° C for 1 hour, 161 g (2.37 mol) of imidazole in 0.7 l of THF are added dropwise in the course of 60 min. After a further 15 min, the mixture is filtered, the solid is washed with 0.5 l of THF, and the filtrate is concentrated to a volume of 1 l, filtered again, then completely concentrated, allowed to stand overnight at 0° C. under argon and again filtered through a frit.

1. waitAfter a further 15 min
2. filtrationthe mixture is filtered
3. washthe solid is washed with 0.5 l of THF
4. concentrationthe filtrate is concentrated to a volume of 1 l
5. filtrationfiltered again
6. concentrationcompletely concentrated
7. waitto stand overnight at 0° C. under argon
8. filtrationagain filtered through a frit