Benzoyl Peroxide → 2-(Bromomethyl)-7-chloro-1,3-benzothiazole
反応式
[Cl:1][C:2]1[C:10]2[S:9][C:8]([CH3:11])=[N:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[Br:12]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:12][CH2:11][C:8]1[S:9][C:10]2[C:2]([Cl:1])=[CH:3][CH:4]=[CH:5][C:6]=2[N:7]=1参加物
5
実験手順
A mixture of 7-chloro-2-methyl-benzothiazole (1.00 g, 5.45 mmol), N-bromosuccinimide (1.26 g, 7.08 mmol), benzoyl peroxide (0.1 g), and CCl4 (10 mL was heated to reflux under irradiation of a UV lamp for 14 h. The reaction mixture was cooled and filtered to remove the succinimide formed in the reaction, and the filtrate was evaporated to dryness. The resulting solid was purified by flash chromatography to give the title lamp (400 mg, 1.5 mmol). 1H-NMR (CDCl3): δ 7.94 (d, 1H), 7.47 (t, 1H), 7.42 (d, 1H), 4.82 (s, 2H, CH2). HPLC Rt: 7.19 min.
後処理
- temperaturewas heated
- temperatureto reflux under irradiation of a UV lamp for 14 h
- temperatureThe reaction mixture was cooled
- filtrationfiltered
- customto remove the succinimide
- customformed in the reaction
- customthe filtrate was evaporated to dryness
- customThe resulting solid was purified by flash chromatography
- customto give the title lamp (400 mg, 1.5 mmol)
出典と根拠
- ORDレコード
- ord-a139d2f85fc1428581b4d72518d71dd6
- 出典データセット
- uspto-grants-2006_11
- 特許番号
- US07138401B2
反応ノート
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