関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | tert-Butyl methyl ether | HCID 15413 | — |
| 反応物 | HCID 86343656 | HCID 86343656 | — |
| 生成物 | 2,4,5-Trifluorophenylacetic acid | HCID 2777950 | 25% |
反応手順
50 ml of concentrated sulphuric acid was added to 1-chloroethynyl-2,4,5-trifluorobenzene of formula IV, X=Cl and the mixture heated to 100° C. and left to stir for 1 hour. 50 ml of MTBE and 100 ml of water were then added. The phases were separated and the aqueous phase was re-extracted with 2×50 ml of MTBE. The combined organic phases were counter extracted with 3×50 ml of aqueous NaHCO3 and put to one side. The three aqueous phases of NaHCO3 were recombined and the resulting phase was acidified with hydrochloric acid and then extracted with 3×50 ml of MTBE. The organic phases were concentrated to a residue obtaining 0.25 g of 2,4,5-trifluorophenylacetic acid of formula (I) with a molar yield of 25%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09238613B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-595be5e545694559902aec5983a04aa2 |
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| 出典メモ | uspto-grants-2016_01 |
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