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Ethanol → 4-amino-4-methyl-N-(2-pyrimidinyl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloropyrimidine | HCID 74404 | — |
| 反応物 | 4-Methylpiperidin-4-amine | HCID 21090445 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-amino-4-methyl-N-(2-pyrimidinyl)piperidine | HCID 21882566 | 65.1% |
反応手順
2 ml of an ethanol suspension containing 260 mg of 4-amino-4-methylpiperidine (synthesized according to a method described in U.S. Pat. No. 5,821,240), 237 mg of 2-chloropyrimidine and 858 mg of potassium carbonate was stirred at 50° C. for 12 hours. The reaction mixture was poured into water, and extracted with chloroform. The extract was washed with brine, dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure. The residue was purified by silica gel flash column chromatography [solvent: chloroform-methanol-aqueous ammonia (300:10:1)] to obtain 259 mg of 4-amino-4-methyl-N-(2-pyrimidinyl)piperidine (Reference Example 8-1 in Table 9).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07332487B2 |
| 出典データセット | uspto-grants-2008_02 |
| ORD ID | ord-a09c43af4c764edeb673678484eda59f |
| 出典メモ | uspto-grants-2008_02 |