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3-Methylpiperidine → 4-(2-Butynyloxy)-5-fluoro-6-(3-methylpiperidino)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Methylpiperidine | HCID 79081 | — |
| 反応物 | 4-(2-Butynyloxy)-5-fluoro-6-chloropyrimidine | HCID 22599717 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(2-Butynyloxy)-5-fluoro-6-(3-methylpiperidino)pyrimidine | HCID 59341133 | 94% |
反応手順
Into 3 ml of ethanol was resolved 0.3 g of 4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine, 0.45 g of 3-methylpiperidine was added therein, and the mixture was stirred for 10 hours under reflux condition. The reaction mixture was cooled to near room temperature, and concentrated. Into the residue was added a saturated ammonium chloride aqueous solution, 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 0.37 g of 4-(2-butynyloxy)-5-fluoro-6-(3-methylpiperidino) pyrimidine (hereinafter, referred to as Compound (3)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732448B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-8cddd482958c467aa020aef6bd39fac4 |
| 出典メモ | uspto-grants-2010_06 |