Bromotrimethylsilane → 1,5-Dibromo-2,3-dihydro-1H-indene
反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[CH:7](O)[CH2:6][CH2:5]2.[Br:12][Si](C)(C)C>C(Cl)(Cl)Cl>[Br:12][CH:7]1[C:8]2[C:4](=[CH:3][C:2]([Br:1])=[CH:10][CH:9]=2)[CH2:5][CH2:6]1参加物
4
実験手順
To a nitrogen-purged flask was added 100 mg (0.469 mmol) of 5-bromoindan-1-ol from Step A and 3 mL of anhydrous chloroform, followed by 0.096 mL (0.704 mmol) of bromotrimethylsilane. The reaction mixture was stirred at ambient temperature overnight and concentrated. The residue was partitioned between ethyl acetate and water. The organic phase was washed with saturated aqueous sodium chloride solution, dried over sodium sulfate, and concentrated to give a brown oil which was used without further purification. Mass spectrum (MS): m/z 195, 197 (M+1-HBr), 116 (M+1-2HBr).
後処理
- customTo a nitrogen-purged flask
- concentrationconcentrated
- customThe residue was partitioned between ethyl acetate and water
- washThe organic phase was washed with saturated aqueous sodium chloride solution
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customto give a brown oil which
- customwas used without further purification
出典と根拠
- ORDレコード
- ord-ec62b51a66dc43eda88977270131fa42
- 出典データセット
- uspto-grants-2007_07
- 特許番号
- US07238683B2
反応ノート
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