化工社化工社 化学情報印刷レポート · 研究参考用
Methylurea → 1,6-Dimethyluracil
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylurea | HCID 11719 | — |
| 反応物 | Diketene | HCID 12661 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1,6-Dimethyluracil | HCID 10606818 | 18% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440983B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-3676721470164f839a71b8ed5c811bf2 |
| 出典メモ | uspto-grants-2016_09 |