関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3,5-Dichloro-2,6-difluoropyridine | HCID 643277 | — |
| 溶媒 | Ethylene Glycol | HCID 174 | — |
| 生成物 | 4-(3,5-Dichloro-6-fluoro-2-pyridyloxy)-2-buten-1-ol | HCID 53655497 | — |
反応手順
To a solution of 11 grams (0.06 mole) of 3,5-dichloro-2,6-difluoropyridine in 35 milliliters of ethylene glycol was added over a 15 minute period 2.44 grams of sodium hydroxide in 35 milliliters of butenediol(2-butene-1,4-diol). The mixture was heated to ~70° C. and agitated for ~31/2 hours. Thereafter the mixture was poured into water and extracted with hot hexane. Most of the hexane was removed and upon cooling the 4-(3,5-dichloro-6-fluoro-2-pyridyloxy)-2-buten-1-ol product precipitated out. The product was recovered in a yield of 9 grams (60 percent of theoretical) and melted at 30° C. Upon analysis, the product was found to have carbon, hydrogen, chlorine and nitrogen contents of 43.3, 2.8, 27.8 and 5.6 percent, respectively, as compared with the theoretical contents of 42.9, 3.2, 28.1 and 5.6 percent, respectively, as calculated for the above named structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04180395 |
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| 出典データセット | uspto-grants-1979_12 |
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| ORD ID | ord-3a3da65924804d2eadbc59d275403fa2 |
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| 出典メモ | uspto-grants-1979_12 |
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