반응 #88617

반응 방정식

1-methylurea

4-methyleneoxetan-2-one

→

1,6-dimethylpyrimidine-2,4(1H,3H)-dione

수율 18.0%

용매

MeOH

반응 조건

후처리

1. 1
   여과The reaction was filtered
2. 2
   세척the filtered solid was washed with MeOH (20 mL)
3. 3
   기타dried

실험 절차

A solution of 1-methylurea (30 g, 0.356 mol) in 4-methyleneoxetan-2-one (26.4 g, 0.356 mol) was heated at 100° C. for 18 h, cooled to RT then diluted with MeOH (50 mL). The reaction was filtered and the filtered solid was washed with MeOH (20 mL) and dried to give 1,6-dimethylpyrimidine-2,4(1H,3H)-dione (9 g, 18% yield) as a white solid. 1H NMR (CDCl3) δ: 8.33 (s, 1H), 5.58 (s, 1H), 3.38 (s, 3H), 2.26 (s, 3H). LCMS: MH+ 141 and TR=0.368 min. Used without further purification.

출처