N-bromobutanimide → 3-(Bromomethyl)benzene-1-sulfonyl chloride
反応式
[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]=1参加物
5
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-aef9790ddf794e36b75a7741f6445f7c
- 出典データセット
- uspto-grants-2010_03
- 特許番号
- US07678794B2
反応ノート
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