関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-Bromoanisole | HCID 16971 | — |
| 反応物 | 4-Fluorobenzoyl chloride | HCID 67879 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | (4-Bromo-2-methoxyphenyl)(4-fluorophenyl)methanone | HCID 59814869 | 18.3% |
反応手順
To a suspension of AlCl3 (14.7 g, 110 mmol) in 250 mL of 1,2-dichloroethane was added 4-fluorobenzoyl chloride (11.8 mL, 100 mmol) at rt. The resulting mixture was stirred at rt for 15 min. and 3-bromoanisole (16.8 g, 90.0 mmol) in 20 mL of 1,2-dichloroethane was added. After 1 h at rt, the brown solution was poured into ice. 2N HCl was added to the aqueous layer followed by an extraction with CH2Cl2. The combined organics were dried (MgSO4), filtered and concentrated. The residue was subjected to chromatography on silica gel (EtOAc/hexane 5:95 to 7:93) affording 5.1 g of a solid that was triturated with 20 mL of EtOAc/hexane (10:90). The title compound was obtained from filtration, and additional product was recovered from the mother liquors.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07439260B2 |
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| 出典データセット | uspto-grants-2008_10 |
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| ORD ID | ord-bc439dbf08e24a499e1b74945d71ca24 |
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| 出典メモ | uspto-grants-2008_10 |
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