反应详情

22.0 g of 7,7,8,9,9-pentamethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione and 5.1 g of potassium hydroxide were added to 200 ml of N,N-dimethylformamide, and the mixture was heated, with stirring, for 30 minutes at 50°-60° C. At the end of this time, 9.0 g of 1,3-dibromo-2-propanol were added dropwise to the mixture and the whole mixture was heated, with stirring, for 6 hours at 100°-110° C. After completion of the reaction, the reaction mixture was condensed by evaporation and the residue was washed with a 1% w/w aqueous solution of potassium hydroxide and then recrystallised from a 2:1 by volume mixture of benzene and ethanol, giving the desired Compound No. 164 in the form of white crystals, melting point 255°-256° C.

1. temperaturethe mixture was heated
2. temperaturethe whole mixture was heated
3. stirringwith stirring, for 6 hours at 100°-110° C
4. customAfter completion of the reaction
5. customcondensed
6. customby evaporation
7. washthe residue was washed with a 1% w/w aqueous solution of potassium hydroxide
8. customrecrystallised from a 2:1 by volume mixture of benzene and ethanol