780800-88-6 → HCID 86594752、化合物
反応式
[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]参加物
4
実験手順
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).
後処理
- filtrationfiltered through celite
- concentrationThe filtrate was concentrated in vacuo
- customto give a yellow oil
- customPurification via column chromatography on silica gel (CH2Cl2
出典と根拠
- ORDレコード
- ord-b20e34de24f646e7b3687d0609b19e55
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07863293B2
反応ノート
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