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Diisopropylamine → 4-(3,5-Dichloro-phenyl)-3-butyn-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | Butyn-2-one | HCID 15018 | — |
| 反応物 | 1,3-Dichloro-5-iodobenzene | HCID 76424 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(3,5-Dichloro-phenyl)-3-butyn-2-one | HCID 18522451 | — |
反応手順
To a solution of 1,3-dichloro-5-iodo-benzene (3.44 g, 12.6 mmol) in THF (220 mL) was added PdCl2(PPh3)2 (904 mg, 1.29 mmol), 3-butyn-2-one (2.18 g, 32.0 mmol), copper(l)iodide (380 mg, 2 mmol) and diisopropylamine (44 mL). The reaction mixture was stirred at room temperature for 48 hours, filtered and evaporated. The residue was purified by column chromatography using methylene chloride:hexanes (1:1) as eluent. The desired 4-(3,5-dichloro-phenyl)-3-butyn-2-one product was isolated in 977 mg yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06569901B2 |
| 出典データセット | uspto-grants-2003_05 |
| ORD ID | ord-460b9aa8d211412dbde382390db9e230 |
| 出典メモ | uspto-grants-2003_05 |