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Potassium Carbonate → (5-Methyl-2-nitro-4-trifluoromethyl-phenyl)-carbamic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Trimethylboroxine | HCID 574072 | — |
| 反応物 | (5-Chloro-2-nitro-4-trifluoromethyl-phenyl)-carbamic acid tert-butyl ester | HCID 69489376 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | (5-Methyl-2-nitro-4-trifluoromethyl-phenyl)-carbamic acid tert-butyl ester | HCID 69486745 | 69% |
反応手順
To a suspension of (5-chloro-2-nitro-4-trifluoromethyl-phenyl)-carbamic acid tert-butyl ester (Example A1) (5.00 g, 14.7 mmol), tetrakis(triphenylphosphine)palladium (1.70 g, 1.47 mmol) and potassium carbonate (6.09 g, 44.1 mmol) in dioxane/water (9:1; 50 ml) was added at RT trimethylboroxine (2.04 ml, 14.7 mmol). The reaction mixture was stirred under reflux conditions for 15 h, filtered, evaporated and purified by column chromato-graphy on silica gel (hexane/ethyl acetate 9:1) to yield a light yellow solid (3.25 g, 69%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06949542B2 |
| 出典データセット | uspto-grants-2005_09 |
| ORD ID | ord-ee5c48acfd834cae99be628d3acedf64 |
| 出典メモ | uspto-grants-2005_09 |