Methanol → 4-(2,3-Dihydroxypropyl)-3-methoxybenzonitrile
反応式
[CH2:1]([C:4]1[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[CH:6][C:5]=1[O:12][CH3:13])C=C.C[N+]1([O-])CC[O:18][CH2:17]C1.[CH3:22][OH:23]>O.O=[Os](=O)(=O)=O>[OH:23][CH:22]([CH2:17][OH:18])[CH2:1][C:4]1[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[CH:6][C:5]=1[O:12][CH3:13]参加物
6
実験手順
To a solution of 4-allyl-3-methoxybenzonitrile (1.1 g, 6.4 mmol) in 30 mL of methanol and 10 mL of water was added OsO4 (140 mg) and NMO (2.2 g, 16 mmol), and the mixture was stirred at ambient temperature overnight. Remove the methanol under reduced pressure, the residue was dissolved in EtOAc, washed with brine, dried over anhydrous sodium sulfate and concentrated. The residue was purified by fast column chromatograph to give 4-(2,3-dihydroxypropyl)-3-methoxybenzonitrile. MS m/z: 208 (M+1)+.
後処理
- customRemove the methanol under reduced pressure
- dissolutionthe residue was dissolved in EtOAc
- washwashed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- customThe residue was purified by fast column chromatograph
出典と根拠
- ORDレコード
- ord-edd16adcc06449d692b2aab77a693426
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09073882B2
反応ノート
読み込み中…