Triphenylphosphine dibromide → HCID 14971319、化合物
反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[O:11][CH2:10][C:9]([CH2:12]O)=[CH:8][C:7]=2[CH:14]=1.[Br:15]P(Br)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>C(#N)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[O:11][CH2:10][C:9]([CH2:12][Br:15])=[CH:8][C:7]=2[CH:14]=1参加物
4
実験手順
6-Methoxy-3-(hydroxymethyl)-2H-1-benzopyran (4.35 g, 22.6 mmol) is dissolved in 70 ml of dry acetonitrile and treated with dibromotriphenylphosphorane (9.56 g, 22.6 mmol). After 15 min, the mixture is evaporated in vacuo. The residue is triturated with 100 ml of an ether/hexane mixture (1:1). The solid is removed by filtration (medium frit) and washed with several 50 ml portions of the ether/hexane mixture. The organic extracts are combined and evaporated to give 6-methoxy-3-(bromomethyl)-2H-1-benzopyran which is used without any further purification.
後処理
- customthe mixture is evaporated in vacuo
- customThe residue is triturated with 100 ml of an ether/hexane mixture (1:1)
- customThe solid is removed by filtration (medium frit)
- washwashed with several 50 ml portions of the ether/hexane mixture
- customevaporated
出典と根拠
- ORDレコード
- ord-d98e93658c5549a4a6365e494319f82a
- 出典データセット
- uspto-grants-1992_10
- 特許番号
- US05155130
反応ノート
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