反应详情

To 3.65 g (32 mmol) of 3-methyl-2,4-pentanedione in ethanol (15 ml) was added urea (1.92 g; 32 mmol) followed by 3 drops concentrated HCl. This mixture was refluxed under N2 overnight (12 hours). Upon cooling a solid separated which was filtered off and washed with cold ethanol and ethyl ether. Drying on the pad gave an off-white tlc pure solid. NMR (d6 -DMSO, δ from TMS): 1.94(S, 5-CH3), 2.22(S, 4, 6 -CH3S), 5.47 (br S, OH). Mass spectroscopy showed M+ at m/e 138.

1. temperatureThis mixture was refluxed under N2 overnight (12 hours)
2. temperatureUpon cooling a solid
3. customseparated which
4. filtrationwas filtered off
5. washwashed with cold ethanol and ethyl ether
6. customDrying on the pad
7. customgave an off-white tlc pure solid