関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,6-Difluoropyridine | HCID 73934 | — |
| 反応物 | 4-Hydroxy-2-(trifluoromethyl)thiophene | HCID 11084273 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Fluoro-6-(2-trifluoromethyl-4-thienyloxy)pyridine | HCID 12115991 | 74.3% |
反応手順
1.00 g of 2,6-difluoropyridine is introduced into 10 ml of DMF under nitrogen and 1.44 g of K2CO3 are added at RT. 1.61 g of 4-hydroxy-2-trifluoromethylthiophene are added and the mixture is heated at 80° C. for 4 h, then cooled to RT and poured into water. After extraction twice with heptane/ethyl acetate (1:1) and twice with ethyl acetate the product is washed with water and saturated sodium chloride solution, dried over MgSO4 and concentrated. Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent gives 1.7 g of 2-fluoro-6-(2-trifluoromethyl-4-thienyloxy)pyridine as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07211673B2 |
|---|
| 出典データセット | uspto-grants-2007_05 |
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| ORD ID | ord-9169015d135343b7bf4f71314f831d37 |
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| 出典メモ | uspto-grants-2007_05 |
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