Dimethylformamide → 2,3-Dichloro-4-(chloromethyl)pyridine
반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([CH2:9]O)[CH:5]=[CH:4][N:3]=1.CN(C=O)C.O=P(Cl)(Cl)[Cl:18]>N#N>[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([CH2:9][Cl:18])[CH:5]=[CH:4][N:3]=1참가 물질
5
실험 절차
(2,3-Dichloro-pyridin-4-yl)-methanol (0.256 g, 1.44 mmol) was dissolved in 5 mL anhydrous under N2. Anhydrous DMF (o. 111 mL, 1.44 mmol) was added followed by dropwise addition of POCl3 (0.134 mL, 1.44 mmol). The reaction was stirred at RT overnight. After 16 h the reaction was quenched by the addition of sat aq NaHCO3. The mixture was extracted 3× with DCM. The organic phases were dried over Na2SO4, filtered, and concentrated to provide the pure titled compound. 1H NMR (CDCl3) δ 8.33 (d, 1H, J=4.9 Hz), 7.44 (d, 1H, J=4.9 Hz), 4.68 (s, 2H).
후처리
- customAfter 16 h the reaction was quenched by the addition of sat aq NaHCO3
- extractionThe mixture was extracted 3× with DCM
- dry with materialThe organic phases were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-441d077c3e984b57b5d127b9e9c915a4
- 출처 데이터셋
- uspto-grants-2003_07
- 특허 번호
- US06586424B2
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