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Potassium Carbonate → 5-[4-(4-fluoro-phenyl)-3,6-dihydro-2H-pyridin-1-ylmethyl]-2-methyl-pyrimidin-4-ylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-(4-Fluorophenyl)-1,2,3,6-tetrahydropyridine hydrochloride | HCID 197747 | — |
| 反応物 | 5-(Chloromethyl)-2-methylpyrimidin-4-amine--hydrogen chloride (1/1) | HCID 21473611 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-[4-(4-fluoro-phenyl)-3,6-dihydro-2H-pyridin-1-ylmethyl]-2-methyl-pyrimidin-4-ylamine | HCID 21473628 | 28% |
反応手順
A suspension of 27.2 g (0.14 mol) of 5-chloromethyl-2-methyl-pyrimidin-4-ylamine hydrochloride, 29.8 g (0.14 mol) of 4-(4-fluoro-phenyl)-1,2,3,6-tetrahydropyridine hydrochloride and 42 g (0.30 mol) of dry potassium carbonate in 200 ml of dimethyl-formamide was stirred at room temperature for 18 hours. The mixture was suction filtered, the filter cake was washed with dichloromethane, the filtrate was completely freed from the solvents and the residue was crystallized twice from ethyl acetate/cyclohexane. 11.6 g (28%) of 5-[4-(4-fluoro-phenyl)-3,6-dihydro-2H-pyridin-1-ylmethyl]-2-methyl-pyrimidin-4-ylamine were obtained as yellowish crystals; m.p. 176°-178°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05688798 |
| 出典データセット | uspto-grants-1997_11 |
| ORD ID | ord-a6b760196417413bb732954c365e53c3 |
| 出典メモ | uspto-grants-1997_11 |