関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Methylphenyl boronic acid | HCID 2733267 | — |
| 反応物 | n-(4-Iodo-6-thiomorpholin-4-yl-pyridin-3-yl)-2,2-dimethyl-propionamide | HCID 22591449 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2,2-Dimethyl-n-(6-thiomorpholin-4-yl-4-o-tolyl-pyridin-3-yl)-propionamide | HCID 22591446 | — |
反応手順
A mixture of 4.05 g (10.0 mmol) N-(4-iodo-6-thiomorpholin-4-yl-pyridin-3-yl)-2,2-dimethyl-propionamide, 54 ml toluene, 16 ml 2 N sodium carbonate solution, 347 mg (0.3 mmol) tetrakis(triphenylphosphine)palladium(0), 67 mg (0.3 mmol) palladium(II) acetate and 1.50 g (11.0 mmol) o-tolylboronic acid was heated under argon at 80° C. for 18 h. After cooling to room temperature, the aqueous phase was separated and washed twice with ethyl acetate. The combined organic layers were washed with 50 ml brine, dried (sodium sulfate) and evaporated. Purification by flash-chromatography gave 3.57 g (quantitative) of the title compound as a light brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06849624B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-cc3b350c60d249e1a0c9ddbd7e0f52b9 |
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| 出典メモ | uspto-grants-2005_02 |
|---|
