Methylurea → 1,6-Dimethyluracil
반응식
[CH3:1][NH:2][C:3]([NH2:5])=[O:4].[CH2:6]=[C:7]1[O:10][C:9](=O)[CH2:8]1>CO>[CH3:1][N:2]1[C:7]([CH3:6])=[CH:8][C:9](=[O:10])[NH:5][C:3]1=[O:4]참가 물질
4
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.
후처리
- filtrationThe reaction was filtered
- washthe filtered solid was washed with MeOH (20 mL)
- customdried
출처 및 근거
- ORD 기록
- ord-3676721470164f839a71b8ed5c811bf2
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09440983B2
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