関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3-Dimethylbenzoic acid | HCID 11782 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Tert-butyl 2-amino-4-(benzo[1,3]dioxol-5-yl)benzoate | HCID 67342168 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Tert-butyl 4-(benzo[1,3]dioxol-5-yl)-2-(2,3-dimethylbenzamido)benzoate | HCID 67342913 | — |
反応手順
1.7 mL of methylene chloride, 1.0 μL N,N-dimethylformamide and 0.025 mL of oxalyl chloride were added to 41 mg of 2,3-dimethylbenzoic acid at room temperature sequentially and stirred ad the same temperature for 1 hour. The reaction mixture was added to a mixed solution of 50 mg of tert-butyl 2-amino-4-(benzo[1,3]dioxol-5-yl)benzoate, 2.8 mL of methylene chloride and 0.36 mL of triethylamine and stirred at room temperature for 1 hour. A saturated sodium hydrogen carbonate aqueous solution was added to the reaction mixture, and the organic layer was separated, and the solvent was evaporated under reduced pressure. The obtained residue was purified with silica gel column chromatography [Flash Tube 2008 manufactured by Trikonex Company, eluent; hexane:ethyl acetate=4:1]to obtain tert-butyl 4-(benzo[1,3]dioxol-5-yl)-2-(2,3-dimethylbenzamido)benzoate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07999132B2 |
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| 出典データセット | uspto-grants-2011_08 |
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| ORD ID | ord-34f7e69ca54144a6b2fbb6e009767c56 |
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| 出典メモ | uspto-grants-2011_08 |
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