関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Thiophenol | HCID 7969 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,6-Dichloropyridine | HCID 16989 | — |
| 反応物 | N-Pyridin-4-ylacetamide | HCID 21288 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 2-Chloro-6-(phenylthio)pyridine | HCID 12760118 | — |
| 溶媒 | Sulfolane | HCID 31347 | — |
| 生成物 | 4-Acetamido-1-(6-phenylthio-2-pyridyl)piperidine | HCID 12926617 | 48.5% |
反応手順
A mixture of 9.5 g of 2-chloro-6-(phenylthio) pyridine (b.p. 112° to 116° C./0.01 mm Hg, prepared by reaction of 2,6-dichloropyridine with the sodium salt of thiophenol), 7.8 g of potassium carbonate and 7.6 g of 4-acetamidopyridine in 75 ml of sulfolane is heated to 150° C. with stirring for 50 hours, then the sulfolane is concentrated to 1/5th of its volume, the mixture is poured in 100 ml of water and extraction is effected four times with 150 ml of diethyl ether. The organic phase is washed with water, dried over anhydrous sodium sulfate, concentrated to dryness and the residue is crystallised in 40 ml of ethyl acetate. 6.8 g of 4-acetamido-1-(6-phenylthio-2-pyridyl)piperidine are thus obtained; m.p. 110° to 112° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04409228 |
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| 出典データセット | uspto-grants-1983_10 |
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| ORD ID | ord-617e70658e0147dbba88ec38debf31af |
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| 出典メモ | uspto-grants-1983_10 |
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