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HRID 19615作成日:2026年10月25日

Ammonium Chloride → (E)-1-(3-Bromo-phenyl)-5-methoxy-pent-4-ene-1,3-dione

https://huagongshe.com/reaction/19615

反応式

関与物質

役割名称HCID仕込み量
反応物Ammonium ChlorideHCID 25517—
反応物Benzoyl chloride, 3-bromo-HCID 74377—
反応物3-Buten-2-one, 4-methoxy-HCID 94297—
反応物Lithium HexamethyldisilazideHCID 2733832—
溶媒TetrahydrofuranHCID 8028—
生成物(E)-1-(3-Bromo-phenyl)-5-methoxy-pent-4-ene-1,3-dioneHCID 67318718—

反応条件

温度-70 °C

反応手順

In a 1 ltr flask is cooled a solution of lithium hexamethyldisilazide (65 ml, 1.5 M) in THF (250 ml) to 75 ° C. During a period of 1 h is added 4-methoxy-but-3-en-2-one (7 ml). The mixture is stirred for 1 h at −70° C. A solution of 3-bromobenzoylchloride (6 g) in THF (250 ml) is added to the above mixture during 1 h at −70° C. The resulting mixture is slowly heated to ambient temperature and stirred for 1 h. Subsequently, the mixture is added to a cold aqueous solution of ammonium chloride and the resulting suspension is extracted with ethyl acetate. The organic phase is extracted twice with an aqueous solution of ammonium chloride, dried over sodium sulfate and evaporated. The crude oily product is transferred to the next step without any further purification.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07745446B2
出典データセットuspto-grants-2010_06
ORD IDord-99ee562778c24210ad8e6056e2283f5e
出典メモuspto-grants-2010_06