反应详情

温度

80 °C

The reaction was conducted in a nitrogen atmosphere with the exclusion of moisture. 21.9 g (50 mmole) of compound (52) were added to 5.6 g (50 mmole) potassium tert-butylate in 400 ml toluene. The mixture was stirred for 30 minutes at room temperature and for 1 hour at 80° C., and was subsequently cooled to 60° C. 7.8 g (50 mmole) 1.4-dioxa-spiro[4.5]decan-8-one were added. The mixture was then stirred for 18 hours at 60° C. and cooled. 100 ml water were added drop-wise. The organic phase was separated off, the aqueous phase was extracted twice with toluene and dried over sodium sulphate, and the solvent was removed by distillation. 29 g oil were obtained, which was purified with 1:4 diisopropyl ether/n-hexane on a silica gel column.

1. temperaturewas subsequently cooled to 60° C
2. stirringThe mixture was then stirred for 18 hours at 60° C.
3. temperaturecooled
4. customThe organic phase was separated off
5. extractionthe aqueous phase was extracted twice with toluene
6. dry with materialdried over sodium sulphate
7. customthe solvent was removed by distillation