関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Propanoic acid, 2-(4-hydroxyphenoxy)-, methyl ester | HCID 366926 | — |
| 反応物 | 2,6,7-Trichloroquinoxaline | HCID 10036978 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Propanoic acid, 2-(4-((6,7-dichloro-2-quinoxalinyl)oxy)phenoxy)-, methyl ester | HCID 187100 | — |
反応手順
In a nitrogen atmosphere, a solution of 3.9 g (0.02 mole) methyl 2-(4-hydroxyphenoxy)propanoate in 20 cc of dimethylformamide was added dropwise at about 15° C. to a suspension of 0.8 g sodium hydride in 10 cc dimethylformamide. When the evolution of hydrogen ceased, 4.7 g of (0.02 mole) 2,6,7-trichloroquinoxaline was added and the reaction mixture was heated for 5 hours at ~130° C. Filtering the reaction mixture yielded a small amount of insoluble material. The filtrate was poured into approximately 200 cc of ice-water. Sodium chloride was added to the solution which was then extracted with 1200 cc of ether (4×300). The ethereal extracts were combined and dried over magnesium sulfate. The ether was removed under vacuum and the crude product was crystallized from CH3OH. Yield 2.8 g, m.p. 100°-105°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04609396 |
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| 出典データセット | uspto-grants-1986_09 |
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| ORD ID | ord-838dd883dd6b4c7281091294dd3bc776 |
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| 出典メモ | uspto-grants-1986_09 |
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