Triethylamine → 5-bromo-N-ethyl-N-methylpyrimidine-2-carboxamide
反応式
[Br:1][C:2]1[CH:3]=[N:4][C:5]([C:8](Cl)=[O:9])=[N:6][CH:7]=1.[CH2:11]([N:13](CC)[CH2:14]C)[CH3:12].C(NC)C>ClCCl>[Br:1][C:2]1[CH:3]=[N:4][C:5]([C:8]([N:13]([CH2:11][CH3:12])[CH3:14])=[O:9])=[N:6][CH:7]=1参加物
5
実験手順
5-Bromo-pyrimidine-2-carbonyl chloride (1600 mg, 7.225 mmol) was dissolved in dichloromethane (25 ml) and triethylamine (4.03 ml, 28.9 mmol) was added followed by ethyl-methyl-amine (0.68 mL, 7.92 mmol). The reaction was stirred at room temperature under nitrogen for 16 ours, after which time, LCMS indicated completion. The mixture was diluted with dichloromethane (50 ml) and washed with water (50 ml) followed by 10% citric acid (50 ml) and brine (50 ml). The organic layer was separated and dried over MgSO4, the residue was filtered and the solvent was removed in vacuo to afford the title compound 5-bromo-N-ethyl-N-methylpyrimidine-2-carboxamide (SM-3): (1.4 g, 79.4%) as a brown oil.
後処理
- washwashed with water (50 ml)
- customThe organic layer was separated
- dry with materialdried over MgSO4
- filtrationthe residue was filtered
- customthe solvent was removed in vacuo
出典と根拠
- ORDレコード
- ord-0c14297aed774874a82f544e3ae66413
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08735396B2
反応ノート
読み込み中…