Ammonia → HCID 118598838, 화합물
반응식
[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]=1참가 물질
4
반응 조건
- 온도
- 50 °C
실험 절차
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]+.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-efe57679f7cd47aa8b8f4307b7a3b171
- 출처 데이터셋
- uspto-grants-2016_07
- 특허 번호
- US09382248B2
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