Boron tribromide → 6-Hydroxyisochroman-1-one
反応式
B(Br)(Br)Br.C[O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13](=[O:17])[O:12][CH:11]=[CH:10]2>C(Cl)Cl>[OH:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13](=[O:17])[O:12][CH2:11][CH2:10]2参加物
4
実験手順
A 1M solution of boron tribromide in methylene chloride (101 mL) was added at 0° C. to a solution of 6-methoxy-isochromen-1-one (8.9 g) in methylene chloride (178 mL). Then the ice bath was removed and the reaction mixture was stirred overnight at room temperature. Then the mixture was cooled to 0° C., water was added and the aqueous phase was extracted several times with ethyl acetate. The organic phases were combined, dried over sodium sulfate and the solvent was removed in vacuum. In this way the product was obtained with molecular weight 162.03 (C9H6O3); MS (ESI): 163 (M+H+).
後処理
- customThen the ice bath was removed
- temperatureThen the mixture was cooled to 0° C.
- additionwater was added
- extractionthe aqueous phase was extracted several times with ethyl acetate
- dry with materialdried over sodium sulfate
- customthe solvent was removed in vacuum
- customIn this way the product was obtained with molecular weight 162.03 (C9H6O3)
出典と根拠
- ORDレコード
- ord-66c2ac52b43d4554bf0846769ba756fa
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08822495B2
反応ノート
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