関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | 3-Fluoro-4-nitroanisole | HCID 565654 | — |
| 反応物 | 2-Piperazineacetic acid, 4-(phenylmethyl)-, methyl ester | HCID 15665466 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-(4-Benzyl-1-(5-methoxy-2-nitrophenyl)piperazin-2-yl)acetic acid | HCID 66769807 | — |
反応手順
To a solution of Example 12C (0.907 g, 3.65 mmol) in acetonitrile (11.69 mL) was added 2-fluoro-4-methoxy-1-nitrobenzene (0.50 g, 2.92 mmol) and potassium carbonate (2.019 g, 14.61 mmol) in water (2.92 mL) followed by 18-crown-6 (0.039 g, 0.146 mmol), and the mixture was heated with an oil bath at 90° C. (reflux) for 24 hours. The solvent was evaporated and water was added followed by dichloromethane. The water phase was washed three times with dichloromethane to remove starting material and then acidified with 1N HCl until pH=1. The acid product was extracted three times with dichloromethane, dried quickly with sodium sulfate and concentrated to give the title compound. MS (ESI) m/z 386.1 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08846663B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-1a25bfed7a854408a47cbd41ae7cce3d |
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| 出典メモ | uspto-grants-2014_09 |
|---|
