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HRID 19614作成日:2026年10月23日

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

https://huagongshe.com/ja/reaction/19614

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4-Iodobenzoyl chlorideHCID 74373—
反応物3-Buten-2-one, 4-methoxy-HCID 94297—
反応物Lithium HexamethyldisilazideHCID 2733832—
溶媒TetrahydrofuranHCID 8028—
生成物1-(4-Iodo-phenyl)-5-methoxy-pent-4-ene-1,3-dioneHCID 67318321—

反応条件

温度-70 °C

反応手順

In a 1 ltr flask is cooled a solution of lithium hexamethyldisilazide (50 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 (6 ml). The mixture is stirred for 1 h at −70° C. A solution of 4-iodobenzoylchloride (7.2 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-da88ff71f72f4a34b33a1f2096cda387
出典メモuspto-grants-2010_06