関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-benzyl-N-methylpiperidin-4-amine | HCID 4136128 | — |
| 反応物 | 1-(6-Chloropyrimidin-4-yl)-5-(methylsulfonyl)indoline | HCID 59566526 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | HCID 86761923 | HCID 86761923 | — |
反応手順
A mixture of 7b (0.14 g, 2.1 eq), 6a (0.1 g, 0.3 mmol) and potassium carbonate (0.1 g, 2.2 eq) in 1 mL of DMA was heated up to 90° C. for 48 h then cooled down to room temperature and diluted with DCM (2 mL) and brine (2 mL). The layers were separated and the aqueous extracted with DCM (2×2 mL). The combined extracts were washed with brine (2×50 mL), dried over magnesium sulfate, filtered and evaporated. The residue was diluted with acetonitrile and purified on preparative HPLC to afford 7c.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08481731B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-94807e5ba900447ca162d4865b48c8e6 |
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| 出典メモ | uspto-grants-2013_07 |
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