反应详情

Metal sodium (23.8 g, 1.034 mol) was reacted with anhydrous ethanol (500 ml). To the clear obtained solution, was added thiourea (54.35 g, 714 mmol) and ethyl 3-methyl-2(3,5-dimethylphenylacetyl)butanoate (13.14 g, 47.6 mol). The reaction medium was maintained under reflux for 6 h, and then was concentrated in vacuo at 40.50° C. To the obtained residue was added concentrated hydrochloric acid (100 ml) and then the solution was brought to pH 4 with acetic acid. The obtained 6-dimethylbenzyl-5-isopropyl-2-thiouracil was dissolved in an aqueous 10% chloroacetic acid solution (200 ml) and the solution was maintained under reflux for 24 h and then cooled to ambient temperature and the obtained precipitates were separated by filtration and washed with cold ethanol and then with ether, and then dried in vacuo at 40° C. to give 6-(3,5-dimethylbenzyl)-5-isopropyluracil (7 g, 54%). Melting point: 213-214° C.

1. temperatureThe reaction medium was maintained
2. temperatureunder reflux for 6 h
3. concentrationwas concentrated in vacuo at 40.50° C
4. additionTo the obtained residue was added concentrated hydrochloric acid (100 ml)
5. dissolutionThe obtained 6-dimethylbenzyl-5-isopropyl-2-thiouracil was dissolved in an aqueous 10% chloroacetic acid solution (200 ml)
6. temperaturethe solution was maintained
7. temperatureunder reflux for 24 h
8. customthe obtained precipitates
9. customwere separated by filtration
10. washwashed with cold ethanol
11. dry with materialwith ether, and then dried in vacuo at 40° C.