反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:8])=[N:6][CH:7]=1.[Br:9]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:9][CH2:8][C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:7][N:6]=1参加物
5
実験手順
To a solution of 5-fluoro-2-methyl-pyridine (0.75 g) (J. Med. Chem. 1989, 32, 1970) in CCl4 (25 ml) is added N-bromosuccinimide (0.96 g; 5.4 mmol) and benzoyl peroxide (200 mg; 0.8 mmol). The mixture is heated at reflux for 3 h, cooled to RT and stirred for additional 12 h. The suspension is filtered through celite and the filtrate is washed with Na2SO4, dried over MgSO4 and evaporated. The crude material (0.22 g) containing approximately 50% of the dibrominated species is used without further purification.
後処理
- temperatureThe mixture is heated
- temperatureat reflux for 3 h
- filtrationThe suspension is filtered through celite
- washthe filtrate is washed with Na2SO4
- dry with materialdried over MgSO4
- customevaporated
- additionThe crude material (0.22 g) containing approximately 50% of the dibrominated species
- customis used without further purification
出典と根拠
- ORDレコード
- ord-38844669a7d5413e81148bcc4f606c06
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07714010B2
関連ノート
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