関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4,6-Dichloro-5-fluoropyrimidine | HCID 11286675 | — |
| 反応物 | cis-2,6-dimethylhexahydro-1H-azepine hydrochloride | HCID 66594948 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(6-chloro-5-fluoropyrimidin-4-yl)-cis-2,6-dimethylhexahydro-1H-azepine | HCID 86607463 | 97.2% |
反応手順
Into 3 ml of acetonitrile were added 0.2 g of 4,6-dichloro-5-fluoropyrimidine, 0.50 g of potassium carbonate and 0.27 g of cis-2,6-dimethylhexahydro-1H-azepine hydrochloride, and the mixture was stirred for 2 hours at 60° C. The reaction mixture was cooled to near room temperature, a saturated ammonium chloride aqueous solution was added therein, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.3 g of 1-(6-chloro-5-fluoropyrimidin-4-yl)-cis-2,6-dimethylhexahydro-1H-azepine
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07973028B2 |
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| 出典データセット | uspto-grants-2011_07 |
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| ORD ID | ord-892c068a57ed430b8776c896bd38e198 |
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| 出典メモ | uspto-grants-2011_07 |
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