반응 #477715
ord-c9b84fdae26a4f24a03674ee18264509
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1농축concentrated in vacuo
- 2기타to provide a crude residue
- 3세척washed with saturated sodium bicarbonate aqueous solution (50 mL) and brine (50 mL)
- 4기타The organic layer was separated
- 5건조dried over sodium sulfate
- 6농축concentrated in vacuo
실험 절차
To solution of 3-amino-4-methylpyridine (540.2 mg, 5.0 mmol, 1 equiv) in dichloromethane (20 mL) was added pyridine (0.8 mL, 10.0 mmol, 2 equiv) and acetic anhydride (0.57 mL, 6.0 mmol, 1.2 equiv). The resultant solution was stirred at room temperature for 16 h and concentrated in vacuo to provide a crude residue. The residue was diluted with dichloromethane (200 mL), and washed with saturated sodium bicarbonate aqueous solution (50 mL) and brine (50 mL). The organic layer was separated, dried over sodium sulfate, and concentrated in vacuo to yield 3-acetylamino-4-methylpyridine (400.2 mg) as yellow solid which was used without further purification.