780800-88-6 → HCID 86594752, 화합물
반응식
[CH2:1]([C:5]1[C:6]([CH2:11][OH:12])=[N:7][CH:8]=[CH:9][CH:10]=1)[CH:2]([CH3:4])[CH3:3]>C(Cl)Cl.O=[Mn]=O>[CH2:1]([C:5]1[C:6]([CH:11]=[O:12])=[N:7][CH:8]=[CH:9][CH:10]=1)[CH:2]([CH3:4])[CH3:3]참가 물질
4
실험 절차
MnO2 (2.01 g, 23.2 mmol) was added to a flask containing a solution of (3-isobutyl-pyridin-2-yl)-methanol (383 mg, 2.32 mmol) in CH2Cl2 (15 mL). The black mixture was stirred at room temperature for 22 hours and then filtered through celite. The filtrate was concentrated in vacuo to give a yellow oil. Purification via column chromatography on silica gel (CH2Cl2:MeOH, 97.5:2.5, v/v) afforded 3-isobutyl-pyridine-2-carbaldehyde as an orange oil (344 mg, 91%). 1H NMR (CDCl3) δ 0.93 (d, 6H, J=6.0 Hz), 1.87 (m, 1H), 2.94 (d, 2H, J=6.0 Hz), 7.39 (dd, 1H, J=9.0, 3.0 Hz), 7.60 (d, 1H, J=9.0), 8.67 (d, 1H, J=6.0 Hz), 10.18 (s, 1H).
후처리
- filtrationfiltered through celite
- concentrationThe filtrate was concentrated in vacuo
- customto give a yellow oil
- customPurification via column chromatography on silica gel (CH2Cl2
출처 및 근거
- ORD 기록
- ord-aaa0fe658f554172ab1bb1e5eb2c286c
- 출처 데이터셋
- uspto-grants-2007_11
- 특허 번호
- US07291631B2
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