Carbon Tetrachloride → 2-(1-Chloroethyl)-5-fluoropyridine
반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:21].[F:25][C:26]1[CH:27]=[CH:28][C:29]([CH:32](O)[CH3:33])=[N:30][CH:31]=1.CCCCC>C(Cl)Cl>[Cl:21][CH:32]([C:29]1[CH:28]=[CH:27][C:26]([F:25])=[CH:31][N:30]=1)[CH3:33]참가 물질
6
실험 절차
A mixture of triphenylphospine (0.92 g, 3.5 mmol) and CCl4 (4 mL) was stirred for 10 min. and then a solution of 1-(5-fluoropyridin-2-yl)ethanol (0.25 g, 1.7 mmol) in DCM (2 mL) was added. After 18 h, pentane (20 mL) was added, the solid material was removed by filtration and the filtrate was concentrated in vacuo. The residue was purified by flash column chromatography (eluent heptane:ethyl acetate 3:1) affording the title compound (8 mg, 3% yield).
후처리
- waitAfter 18 h
- customthe solid material was removed by filtration
- concentrationthe filtrate was concentrated in vacuo
- customThe residue was purified by flash column chromatography (eluent heptane:ethyl acetate 3:1)
출처 및 근거
- ORD 기록
- ord-af6820bd0fc746cd96180bbe93fcc51e
- 출처 데이터셋
- uspto-grants-2012_04
- 특허 번호
- US08158785B2
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