反应详情

To a solution of 10 g (199.76 mmol) acetylacetone in THF at room temperature loaded with 20 g of Na2SO4 was added 24.49 g (239.71 mmol) 1-dimethylamino-2-propylamine. The slurry was stirred for 16 hours at room temperature and reaction deemed to be complete by GC/MS. All volatiles were evaporated off under vacuum and unreacted acetylacetone and diamine were removed by heating at 60° C. under 100 mTorr vacuum for 2 hours. Yellow residual oil was purified via vacuum transfer heating at 130° C. under 100 mTorr vacuum. 13.5 g of light yellow oil was obtained as pure product with a yield of 74%.

1. customat room temperature
2. customreaction
3. customAll volatiles were evaporated off under vacuum and unreacted acetylacetone and diamine
4. customwere removed
5. temperatureby heating at 60° C. under 100 mTorr vacuum for 2 hours
6. customYellow residual oil was purified via vacuum transfer
7. temperatureheating at 130° C. under 100 mTorr vacuum