Water → HCID 86660229、化合物
反応式
[Br:1][C:2]1[C:7]([NH2:8])=[CH:6][N:5]=[CH:4][N:3]=1.CC(C)([O-])C.[Na+].I[CH2:16][CH2:17][CH2:18][CH3:19].O>CC(N(C)C)=O>[Br:1][C:2]1[C:7]([NH:8][CH2:16][CH2:17][CH2:18][CH3:19])=[CH:6][N:5]=[CH:4][N:3]=1参加物
6
反応条件
- 温度
- 60 °C
実験手順
A mixture of 4-bromopyrimidin-5-amine (1 g, 5.75 mmol), sodium tert-butoxide (1.11 g, 11.5 mmol) and 1-iodobutane (1.11 g, 6.03 mmol) in DMA (15 mL) was heated at 60° C. for 15 hours. The mixture was poured into water and extracted with ethyl acetate. The acetate layer was washed with water, brine, dried with MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by chromatography (hexanes-EtOAc 3:1) to afford 300 mg of the title compound. MS (ESI) m/z 230 (M+H)+.
後処理
- extractionextracted with ethyl acetate
- washThe acetate layer was washed with water, brine
- dry with materialdried with MgSO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was purified by chromatography (hexanes-EtOAc 3:1)
出典と根拠
- ORDレコード
- ord-509645f6c45b4840ad0ef5bbfb32b402
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08586596B2
反応ノート
読み込み中…