Sodium Cyanide → 5-Bromopyrimidine-2-carbonitrile
反応式
[C-]#N.[Na+].C1N2CC[N:6](CC2)[CH2:5]1.[Br:12][C:13]1[CH:14]=[N:15][C:16](Cl)=[N:17][CH:18]=1>CS(C)=O.O>[Br:12][C:13]1[CH:14]=[N:15][C:16]([C:5]#[N:6])=[N:17][CH:18]=1参加物
6
実験手順
To a solution of NaCN (0.849 g, 17.32 mmol) and DABCO (0.390 g, 3.48 mmol) in a mixture of DMSO (4 ml) and H2O (9 ml) was added a solution of 5-bromo-2-chloropyrimidine (3.05 g, 15.75 mmol) in DMSO (9 ml). The solution was stirred at room temperature overnight, and then diluted with water, and extracted with EtOAc. The combined organic layer was dried over anhydrous Na2SO4 and concentrated to give 5-bromopyrimidine-2-carbonitrile (2.327 g, 12.01 mmol, 76% yield, 1H NMR (CDCl3 500 MHz): δ 8.94 (s, 2H)).
後処理
- extractionextracted with EtOAc
- dry with materialThe combined organic layer was dried over anhydrous Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-fd48237f294746c798ba3a3ce2577919
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09108938B2
反応ノート
読み込み中…