関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1,1-Difluoro-2,2-dimethyl-3-[3-(N-phenyl-N-acetylamino)-4-fluorobenzyloxy]propane | HCID 21281089 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 21281080 | HCID 21281080 | 52% |
反応手順
1,1-Difluoro-2,2-dimethyl-3-[3-(N-phenyl-N-acetylamino)-4fluorobenzyloxy]propane (0.5 g) was suspended in a 1 molar solution of potassium hydroxide in water containing 20% by volume ethanol and the mixture was heated at the reflux temperature for 8 hours. After standing overnight at the ambient temperature, the mixture was shaken several times with ethyl acetate and the combined organic extracts washed with water and brine, and dried over anhydrous magnesium sulphate. Evaporation of the solvent under reduced pressure gave a brown oil which was purified by column chromatography on a silica gel supoort, eluting with petroleum ether (boiling range 40°-60° C.) containing 10% by volume ethyl acetate, to give the title compound (0.23 g) as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04792563 |
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| 出典データセット | uspto-grants-1988_12 |
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| ORD ID | ord-a97baa1ff93c429eb52f47454fbbfa89 |
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| 出典メモ | uspto-grants-1988_12 |
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