N-bromobutanimide → 3-(Bromomethyl)benzene-1-sulfonyl chloride
반응식
[Br:1]N1C(=O)CCC1=O.[CH3:9][C:10]1[CH:11]=[C:12]([S:16]([Cl:19])(=[O:18])=[O:17])[CH:13]=[CH:14][CH:15]=1>C(Cl)(Cl)(Cl)Cl.CC(N=NC(C#N)(C)C)(C#N)C>[Br:1][CH2:9][C:10]1[CH:11]=[C:12]([S:16]([Cl:19])(=[O:18])=[O:17])[CH:13]=[CH:14][CH:15]=1참가 물질
5
실험 절차
Add N-bromosuccinimide (9.34 g, 52.5 mmol) and AIBN (5 mg, 0.32 mmol) to a solution of 3-methyl-benzenesulfonyl chloride (10.0 g, 52.5 mmol) in carbon tetrachloride (52 mL), and heat the solution at reflux for 12 hours. Filter the mixture to remove solids and condense under reduced pressure to afford a thick oil. Purify by flash chromatography to yield the title compound as an off-white crystalline solid (5.24 g, 19.4 mmol): 1H NMR (CDCl3) δ 4.54 (s, 2H), 7.62 (m, 1H), 7.78 (m, 1H), 7.98 (m, 1H), 8.06 (m, 1H).
후처리
- temperatureheat the solution
- temperatureat reflux for 12 hours
- filtrationFilter the mixture
- customto remove
- customsolids and condense under reduced pressure
- customto afford a thick oil
- customPurify by flash chromatography
출처 및 근거
- ORD 기록
- ord-aef9790ddf794e36b75a7741f6445f7c
- 출처 데이터셋
- uspto-grants-2010_03
- 특허 번호
- US07678794B2
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