반응식
C([O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH3:12])[N:7]=1)(=O)C.Cl>CO>[OH:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH3:12])[N:7]=1참가 물질
4
실험 절차
2-Acetoxymethyl-6-methylpyridine (5 g) was added to saturated hydrochloric acid in methanol (250 ml, prepared by adding 25 ml of acetyl chloride to 225 ml of methanol). The reaction mixture was stirred at room temperature for 18 hours. The solvent was removed under vacuum and the residue was dissolved in dichloromethane (100 ml) and washed with 2N sodium hydroxide solution (3×50 ml). The combined organic layers were washed with brine (1×200 ml), then dried (MgSO4), filtered and evaporated to give the required product as an oil (2.6 g). 1H NMR (250 MHz, CDCl3) δ 2.54 (3H, s), 3.80 (1H, bs), 4.72 (2H, s), 7.04 (2H, d, J=7.7Hz), 7.57 (1H, t, J=7.7Hz).
후처리
- customThe solvent was removed under vacuum
- dissolutionthe residue was dissolved in dichloromethane (100 ml)
- washwashed with 2N sodium hydroxide solution (3×50 ml)
- washThe combined organic layers were washed with brine (1×200 ml)
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated
출처 및 근거
- ORD 기록
- ord-55e5b9c5717b4ade9770157e506a096b
- 출처 데이터셋
- uspto-grants-2001_07
- 특허 번호
- US06255305B1
연결된 노트
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