関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acrylate | HCID 8821 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | t-Butyl [2-(5-cyano-2-iodophenoxy)ethyl]carbamate | HCID 11111864 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 3-[2-(2-(t-butoxycarbonylamino)ethoxy)-4-cyanophenyl]acrylate | HCID 69921285 | — |
反応手順
11.0 g (28.4 mmol) of 3-[2-(t-butoxycarbonylamino)ethoxy]-4-iodobenzonitrile was dissolved in 200 ml of DMF. 15.4 ml (142 mmol) of ethyl acrylate, 20 ml (142 mmol) of triethylamine and 127 mg (0.567 mmol) of palladium acetate were added to the obtained solution. They were stirred at 100° C. overnight and then treated with ethyl acetate as the extraction solvent in an ordinary manner to obtain the crude product. After the purification by the silica gel column chromatography, the title compound was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06812231B2 |
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| 出典データセット | uspto-grants-2004_11 |
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| ORD ID | ord-6fcd5222fd0b47fe8a222238ed191871 |
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| 出典メモ | uspto-grants-2004_11 |
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