化工社化工社 化学情報印刷レポート · 研究参考用
Water → Methyl 6-(2,2,2-trifluoroethoxy)picolinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-(2,2,2-Trifluoroethoxy)pyridine-2-carboxylic acid | HCID 21253041 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | Methyl 6-(2,2,2-trifluoroethoxy)picolinate | HCID 67510684 | 45% |
反応手順
A mixture of 6-(2,2,2-trifluoroethoxy)picolinic acid (2.40 g, 10.9 mmol, Step-1), methyl iodide (3.39 mL, 54.3 mmol) and potassium carbonate (4.50 g, 32.6 mmol) in N,N-dimethylacetamide (54 mL) is stirred at room temperature for 4 hours. The reaction mixture is poured into water (100 mL) and extracted with n-hexane/ethyl acetate (1:10, 100 mL). The organic layer is washed with water (100 mL), dried over sodium sulfate, and concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (5:1) to give 1.14 g (45% yield) of the title compound as colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09302991B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-cda06d7b6082405999f359872291792b |
| 出典メモ | uspto-grants-2016_04 |