関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Fluoroaniline | HCID 9731 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Phosphine, tris(4-methoxyphenyl)- | HCID 70071 | — |
| 反応物 | 2-Chloro-6-[3-(trifluoromethyl)phenoxy]pyridine | HCID 11011172 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Methylcyclohexane | HCID 7962 | — |
| 生成物 | Picolinafen | HCID 3294375 | — |
反応手順
Analogously to Example 4, 6.84 g (25 mmol) of 2-chloro-6-[3-(trifluoromethyl)phenoxy]pyridine, 3.33 g (30 mmol) of 4-fluoroaniline, 2.92 g (27.5 mmol) of sodium carbonate, 5.6 mg (25 μmol) of palladium(II) acetate and 260 mg (0.75 mmol) of tris(4-methoxyphenyl)phosphine in 25 ml of methylcyclohexane were reacted under a CO pressure of 7.5 bar for 20 hours. After cooling to 80° C., the reaction mixture was diluted with 65 ml of warm methylcyclohexane. The salts were filtered off and washed with 10 ml of warm methylcyclohexane. On cooling to 5° C. the product crystallized. The yield was 8.1 g (86 percent) of a light beige solid. The melting point was 104.5° to 105.1° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06271372B1 |
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| 出典データセット | uspto-grants-2001_08 |
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| ORD ID | ord-16662f582fef43ff9c8839a9a1b97838 |
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| 出典メモ | uspto-grants-2001_08 |
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