Benzoyl Peroxide → HCID 55298631, 화합물

HRID 426243노트

반응식

HRID 426243 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 55298631HCID 55298631, 화합물수율 13.6%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-3b0e6d11dd89466a9b788deb3ede8fc1
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106064B2

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