Carbon tetrabromide → 3-(Bromomethyl)-2-methoxy-6-methylpyridine
反応式
[CH3:1][O:2][C:3]1[C:8]([CH2:9]O)=[CH:7][CH:6]=[C:5]([CH3:11])[N:4]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:32]>ClCCl>[Br:32][CH2:9][C:8]1[C:3]([O:2][CH3:1])=[N:4][C:5]([CH3:11])=[CH:6][CH:7]=1参加物
5
実験手順
To a solution of (2-methoxy-6-methylpyridin-3-yl)methanol (4.7 g, 30.7 mmol) in dichloromethane (150 mL) was added triphenylphosphine (12.1 g, 46.0 mmol). The mixture was cooled in an ice bath with stirring under an atmosphere of nitrogen. Carbon tetrabromide (15.3 g; 46.0 mmol) was added and the mixture was stirred for 90 minutes. The mixture was concentrated under reduced pressure and purified using column chromatography on silica, eluting with dichloromethane/hexanes (1:1) to give 3-(bromomethyl)-2-methoxy-6-methylpyridine (2.0 g).
後処理
- temperatureThe mixture was cooled in an ice bath
- stirringthe mixture was stirred for 90 minutes
- concentrationThe mixture was concentrated under reduced pressure
- custompurified
- washeluting with dichloromethane/hexanes (1:1)
出典と根拠
- ORDレコード
- ord-465f2463928a465a9694a89a9c7541e9
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08841455B2
反応ノート
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