Ammonia → HCID 118598838、化合物
反応式
[Br:1][C:2]1[C:7](=[O:8])[NH:6][C:5]([C:9]([O:11]CC)=O)=[N:4][CH:3]=1.[NH3:14]>C(O)C>[Br:1][C:2]1[C:7](=[O:8])[NH:6][C:5]([C:9]([NH2:14])=[O:11])=[N:4][CH:3]=1参加物
4
反応条件
- 温度
- 50 °C
実験手順
To a solution of ethyl 5-bromo-6-oxo-1,6-dihydropyrimidine-2-carboxylate (4, 0.2 g, 0.81 mmol) in ethanol (4 mL), liquid ammonia (4 mL) was added dropwise at room temperature. The reaction mixture was heated at 50° C. for 16 h. TLC showed consumption of starting material. Solvent was removed under reduced pressure and the residue was treated with methanol (1 mL) and filtered. The solid was washed with diethyl ether and dried under reduced pressure to afford 5-bromo-6-oxo-1,6-dihydropyrimidine-2-carboxamide (5) as off white solid. Yield: 0.14 g, 76%; MS (ESI) m/z 218.87 [M+1]+.
後処理
- customconsumption of starting material
- customSolvent was removed under reduced pressure
- additionthe residue was treated with methanol (1 mL)
- filtrationfiltered
- washThe solid was washed with diethyl ether
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-efe57679f7cd47aa8b8f4307b7a3b171
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09382248B2
反応ノート
読み込み中…