N-bromobutanimide → 2-Bromomethyl-4-tert-butyl-6-chloro-pyridine
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([CH3:11])([CH3:10])[CH3:9])[CH:5]=[C:4]([CH3:12])[N:3]=1.[Br:13]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl.CC(N=NC(C#N)(C)C)(C#N)C>[Br:13][CH2:12][C:4]1[CH:5]=[C:6]([C:8]([CH3:9])([CH3:11])[CH3:10])[CH:7]=[C:2]([Cl:1])[N:3]=1参加物
5
実験手順
Dissolve 2-chloro-6-methyl-4-tert-butyl-pyridine (3.00 g, 16.33 mmol), N-bromosuccinimide (3.20 g, 17.97 mmol) and AIBN (0.03 g, 0.16 mmol) in carbon tetrachloride (60 mL) and heat to reflux. After heating for 6 hours, stir the contents overnight at ambient temperature. The contents are then concentrated to dryness and dry loaded onto a silica plug and eluted with dichloromethane to obtain the title compound (1.90 g, 7.23 mmol). MS(ES), m/z 263 (M+1).
後処理
- temperatureheat to reflux
- temperatureAfter heating for 6 hours
- concentrationThe contents are then concentrated to dryness
- customdry
- washeluted with dichloromethane
出典と根拠
- ORDレコード
- ord-01f1f9d32d2449c4aa81d10a9882dbd7
- 出典データセット
- uspto-grants-2010_02
- 特許番号
- US07666879B2
反応ノート
読み込み中…