Benzoyl Peroxide → HCID 55298631、化合物

HRID 426243ノート

反応式

HRID 426243 の反応式
[F:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[N:3]=1.[Cl:10]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Cl:10][CH2:8][C:6]1[CH:5]=[C:4]([CH3:9])[N:3]=[C:2]([F:1])[CH:7]=1

参加物

5

反応物 3

HCID 7187Benzoyl PeroxideHCID 31398ChlorosuccinimideHCID 198673702-Fluoro-4,6-dimethylpyridine

生成物 1

HCID 55298631HCID 55298631、化合物収率 13.6%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

2-Fluoro-4,6-dimethyl-pyridine (4.25 g, 34 mmol) was refluxed with N-chlorosuccinimide (4.99 g, 37.4 mmol) and benzoyl peroxide (822 mg, 3.4 mmol) in carbon tetrachloride (70 ml). After 3.5 hr., the mixture was cooled to room temperature and filtered. The filtrate was evaporated in vacuo and the residue was purified by silica gel column chromatography (eluent, ether:hexane (1:30)) to afford 740 mg (13%) of 4-chloromethyl-2-fluoro-6-methyl-pyridine as a yellow oil. 1H NMR (200 MHz, CDCl3) δ 2.51 (3H, s), 4.51 (2H, s), 6.77 (1H, s), 7.05 (1H, s).

後処理

  1. filtrationfiltered
  2. customThe filtrate was evaporated in vacuo
  3. customthe residue was purified by silica gel column chromatography (eluent, ether:hexane (1:30))

出典と根拠

ORDレコード
ord-3b0e6d11dd89466a9b788deb3ede8fc1
出典データセット
uspto-grants-2012_01
特許番号
US08106064B2

反応ノート

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