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HRID 76787作成日:2026年10月25日
1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 5-(tert-Butyl)-3,3-dimethyl-6-nitrobenzofuran-2(3H)-one
https://huagongshe.com/reaction/76787
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 2-(5-Tert-butyl-2-hydroxy-4-nitrophenyl)-2-methylpropanoic acid | HCID 59544150 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-(tert-Butyl)-3,3-dimethyl-6-nitrobenzofuran-2(3H)-one | HCID 59544154 | — |
反応手順
To a solution of compound 18 (7.10 g, 25.2 mmol) in 710 mL of anhydrous THF was added EDCI (14.5 g, 75.6 mmol). The resulting suspension was left stirring at 30° C. overnight. The precipitate was filtered and thoroughly washed with DCM. The filtrate was concentrated to dryness and the residue was dissolved in DCM (100 mL). The solution was washed with water (50 mL×2) and brine (50 mL×1). The DCM layer was then dried over anhydrous Na2SO4 and concentrated to give the crude product, which was purified via column chromatography on silica gel (Petroleum ether/EtOAc 200:1→100:1→50:1) to give compound 19 as a white solid. 1H NMR (CDCl3; 400 MHz) δ 7.36 (s), δ 7.10 (s), δ 1.53 (s), δ 1.41 (s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08835639B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-8c5d57b67594402dbaa9b5e31292693d |
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| 出典メモ | uspto-grants-2014_09 |
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