Benzoyl Peroxide → HCID 19390097, 화합물

HRID 1042357노트

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HRID 1042357 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[O:9][CH3:10].C1C(=O)N([Br:18])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:18][CH2:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[C:3]=1[O:9][CH3:10]

참가 물질

5

실험 절차

A solution of 1-chloro-2-methoxy-3-methyl-benzene (13.40 g, 85.60 mmol), NBS (15.30 g, 86.00 mmol) and a catalytic amount of benzoyl peroxide (150 mg) in CCl4 was refluxed for 30 minutes. The reaction mixture was cooled to room temperature and filtered. The precipitate was washed with pentane. The solvent was distilled off and the residue was purified by column chromatography using pentane as the eluant to afford the title compound. Spectroscopic data: 1H NMR (300 MHz, CDCl3) δ 4.00 (s, 3H), 4.56 (s, 2H), 7.04 (t, J=7.62 Hz, 1H), 7.29 (dd, J=7.62 Hz, 1H), 7.34 (dd, J=7.92 Hz, 1H).

후처리

  1. filtrationfiltered
  2. washThe precipitate was washed with pentane
  3. distillationThe solvent was distilled off
  4. customthe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-91e223c0fc3f4945ad1067a96e327316
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08557853B2

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