Dimethylformamide → 2-Iodo-5-propoxypyridine
반응식
I[CH2:2][CH2:3][CH3:4].[I:5][C:6]1[N:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1.C(=O)(O)[O-].[K+].CN(C=O)C>C(Cl)Cl.O>[I:5][C:6]1[CH:7]=[CH:8][C:9]([O:12][CH2:2][CH2:3][CH3:4])=[CH:10][N:11]=1참가 물질
7
반응 조건
- 온도
- 80 °C
실험 절차
Iodopropane (0.18 mL, 1.8 mmol) was added dropwise to a mixture comprising 6-iodopyridin-3-ol (0.32 g, 1.14 mmol), potassium bicarbonate (0.23 g, 1.7 mmol) and DMF (2 mL). The mixture was heated at 80° C. for 1 hour, cooled and diluted with methylene chloride and water. The aqueous layer was separated and extracted with methylene chloride (20 mL). The combined organic layers were washed with water 30 mL, dried (MgSO4) and concentrated under reduced pressure to provide 2-iodo-5-propoxypyridine. MS (ESI); Calculated for C8H10NIO, 266.1, Found (MH+): 222.
후처리
- temperaturecooled
- customThe aqueous layer was separated
- extractionextracted with methylene chloride (20 mL)
- washThe combined organic layers were washed with water 30 mL
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-83809f9e206d4f349bf62a97ce46f2c2
- 출처 데이터셋
- uspto-grants-2000_11
- 특허 번호
- US06150379
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