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Potassium Carbonate → 4-Acetamido-1-(6-methyl-2-pyridyl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N-Pyridin-4-ylacetamide | HCID 21288 | — |
| 反応物 | 6-Chloro-2-picoline | HCID 87601 | — |
| 溶媒 | Sulfolane | HCID 31347 | — |
| 生成物 | 4-Acetamido-1-(6-methyl-2-pyridyl)piperidine | HCID 12926618 | 28% |
反応手順
0.042 mole of 2-chloro-6-methylpyridine, 0.056 mole of anhydrous potassium carbonate and 0.052 mole of 4-acetamidopyridine in 75 ml of sulfolane are heated to 150° C. with stirring for 24 hours, then the sulfolane is concentrated up to 1.5 of its volume, the mixture is poured into 100 ml of water and extraction is effected four times with 150 ml of diethyl ether. The organic phase is washed with water, it is dried over anhydrous sodium sulfate, concentrated to dryness and the residue is crystallised in 40 m of ethyl acetate. Thus, the 4-acetamido-1-(6-methyl-2-pyridyl)piperidine is obtained; m.p. 145° to 147° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04409228 |
| 出典データセット | uspto-grants-1983_10 |
| ORD ID | ord-a522ec499de54b678a31a66f02df464a |
| 出典メモ | uspto-grants-1983_10 |