Bromine → 4,7-dibromo-3,4-dihydrobenzo[b]oxepin-5(2H)-one
反応式
[Br:1][C:2]1[CH:13]=[CH:12][C:5]2[O:6][CH2:7][CH2:8][CH2:9][C:10](=[O:11])[C:4]=2[CH:3]=1.[Br:14]Br>C(OCC)C>[Br:14][CH:9]1[CH2:8][CH2:7][O:6][C:5]2[CH:12]=[CH:13][C:2]([Br:1])=[CH:3][C:4]=2[C:10]1=[O:11]参加物
4
実験手順
To a solution of 7-bromo-3,4-dihydro-2H-benzo[b]oxepin-5-one (700 mg) in diethyl ether (20 mL) at 0° C. was added bromine (0.14 mL) dropwise and the reaction was stirred at room temperature for 16 h. The reaction was then quenched with aqueous sodium thiosulfate solution (30 mL) and the product extracted into diethyl ether (2×30 mL) The combined organics were dried (MgSO4), reduced in vacuo and purified on silica to give 4,7-dibromo-3,4-dihydro-2H-benzo[b]oxepin-5-one.
後処理
- customThe reaction was then quenched with aqueous sodium thiosulfate solution (30 mL)
- extractionthe product extracted into diethyl ether (2×30 mL) The combined
- dry with materialorganics were dried (MgSO4)
- custompurified on silica
出典と根拠
- ORDレコード
- ord-5e5d1d58b2854329bfb1249dc3093497
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09309265B2
反応ノート
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