関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-(Trifluoromethyl)piperidine | HCID 2760776 | — |
| 反応物 | 4-(2-Butynyloxy)-5-fluoro-6-chloropyrimidine | HCID 22599717 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-(2-Butynyloxy)-5-fluoro-6-(3-methylpiperidino)pyrimidine | HCID 59341133 | 108.6% |
反応手順
Into 2 ml of N,N-dimethylformamide was resolved 0.2 g of 4-(2-butynyloxy)-5-fluoro-6-chloropyrimidine, 0.28 g of potassium carbonate and 0.15 g of 3-trifluoromethylpiperidine was added therein, and the mixture was stirred for 5 hours at 70° C. The reaction mixture was cooled to near room temperature, ethyl acetate was added therein, and the mixture was washed with a saturated sodium chloride aqueous solution three times. The organic layers were dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.28 g of 4-(2-butynyloxy)-5-fluoro-6-(3-methylpiperidino)pyrimidine (hereinafter, referred to as Compound (26)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07732448B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-00f61ddb30bd477ab989cca5baa6be4b |
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| 出典メモ | uspto-grants-2010_06 |
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