반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][N:6]=[C:5]([NH2:9])[CH:4]=1)[CH3:2].Cl[CH2:11][CH:12]=O>CCO>[CH2:1]([C:3]1[CH:8]=[CH:7][N:6]2[CH:11]=[CH:12][N:9]=[C:5]2[CH:4]=1)[CH3:2]참가 물질
4
실험 절차
A mixture of 4-ethylpyridin-2-amine (3.21 g, 8.19 mmol), and chloroacetaldehyde (50% aqueous solution, 2.6 ml, 10.5 mmol) in EtOH (10 ml) was refluxed vigorously for 12 hours. The reaction mixture was concentrated, and the residue was suspended in saturated aqueous sodium bicarbonate solution. The aqueous mixture was extracted with CH2Cl2 and EtOAc, and the combined organic extracts were dried over Na2SO4, filtered and concentrated to afford the desired product (1.18 g, 98% yield) as a viscous oil. MS APCI (+) m/z 147.2 (M+1) detected.
후처리
- temperaturewas refluxed vigorously for 12 hours
- concentrationThe reaction mixture was concentrated
- extractionThe aqueous mixture was extracted with CH2Cl2 and EtOAc
- dry with materialthe combined organic extracts were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-a14ef65495744592aceb2fbe75dcfb13
- 출처 데이터셋
- uspto-grants-2012_03
- 특허 번호
- US08138181B2
연결된 노트
불러오는 중…