Formaldehyde → Methyl 2-(5-(dimethylamino)pyridin-2-yl)acetate
反応式
N[C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([O:11][CH3:12])=[O:10])=[N:6][CH:7]=1.[CH2:13]=O.[BH3-][C:16]#[N:17].[Na+]>CO.CC(O)=O>[CH3:13][N:17]([CH3:16])[C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([O:11][CH3:12])=[O:10])=[N:6][CH:7]=1参加物
6
実験手順
To the solution of methyl 2-(5-aminopyridin-2-yl)acetate (800 mg, 4.8 mmol) and paraformaldehyde (578.3 mg, 19.3 mmol) in methanol (20 mL) was added NaBH3CN (1.2 g, 19.26 mmol) and AcOH (1 drop, cat.). The mixture was stirred at room temperature for 12 h. Then, the reaction was quenched with aqueous ammonium chloride and extracted with DCM. The organic layer was with brine, dried over sodium sulfate and evaporated under reduced pressure. The residue was purified by a standard method to get desired product.
後処理
- customThen, the reaction was quenched with aqueous ammonium chloride
- extractionextracted with DCM
- dry with materialdried over sodium sulfate
- customevaporated under reduced pressure
- customThe residue was purified by a standard method
出典と根拠
- ORDレコード
- ord-d418b8ade1784f5387eee54b70baf3a3
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09029531B2
反応ノート
読み込み中…