Methylurea → 1,6-Dimethyluracil
反応式
[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]参加物
4
実験手順
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.
後処理
- filtrationThe reaction was filtered
- washthe filtered solid was washed with MeOH (20 mL)
- customdried
出典と根拠
- ORDレコード
- ord-3676721470164f839a71b8ed5c811bf2
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09440983B2
反応ノート
読み込み中…