関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Tert-Butyl nitrite | HCID 10906 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | 2-Chloro-3-pyridylamine | HCID 80528 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 2-Chloro-3-(2,2,2-trifluoroethoxy)pyridine | HCID 12056728 | — |
反応手順
A reactor vessel is charged with 3-amino-2-chloropyridine (2.7 g, 21 mmol), 2,2,2-trifluoroethanol (15 g, 150 mmol), and trifluoroacetic acid (3.63 g, 31.8 mmol). The solution is cooled to 15° C. and magnesium sulfate (2.6 g) is charged to the vessel. The reagent t-butyl nitrite (2.51 g of a 96% solution, 23.4 mmol) is added drop-wise to the vessel while maintaining the temperature in the range 15° C. to 20° C. The solution is neutralized with aqueous saturated sodium bicarbonate solution and then extracted with MTBE. The solvent is removed by evaporation to obtain 2-chloro-3-(2,2,2-trifluoroethoxy)pyridine as a crude oil (1.58 g, crude yield 35.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06710180B2 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-d39c4576ec454630a4218cea4eedd2cf |
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| 出典メモ | uspto-grants-2004_03 |
|---|
