Bromine → 5-Bromo-2,3-dihydro-5h-benzo[b]oxepin-4-one
反応式
[O:1]1[CH2:7][CH2:6][C:5](=[O:8])[CH2:4][C:3]2[CH:9]=[CH:10][CH:11]=[CH:12][C:2]1=2.[Br:13]Br>C(OCC)C>[Br:13][CH:4]1[C:5](=[O:8])[CH2:6][CH2:7][O:1][C:2]2[CH:12]=[CH:11][CH:10]=[CH:9][C:3]1=2参加物
4
実験手順
To a solution of 2,3-dihydro-5H-benzo[b]oxepin-4-one (1 eq, 1.6 mmol, 260 mg,), in anhydrous diethyl ether (10 ml), bromine was added dropwise (1.1 eq, 1.76 mmol, 90 ul), and the reaction allowed to stir for an hour. The reaction was absorbed onto silica and purified on the ISCO companion running a gradient from 0% ethyl acetate/petrol to 15% ethyl acetate/petrol, with the product seen at 9% ethyl acetate. This gave 5-bromo-2,3-dihydro-5H-benzo[b]oxepin-4-one as an oil (270 mg, yield 70%).
後処理
- customThe reaction was absorbed onto silica
- custompurified on the ISCO companion
出典と根拠
- ORDレコード
- ord-e3bb94870e13475c9340c236b4864e97
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09309265B2
反応ノート
読み込み中…