関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | 1-Isopropylpiperazine | HCID 78013 | — |
| 反応物 | 2-Chloro-5-(4-chlorophenyl)pyridine | HCID 10036554 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-[5-(4-Chlorophenyl)pyridin-2-yl]-4-(propan-2-yl)piperazine | HCID 15951315 | 85.2% |
反応手順
A mixture of 2-chloro-5-(4-chlorophenyl)pyridine (500 mg, 2.23 mmol), DMSO (2.0 mL) and 1-isopropylpiperazine (3 mL, 23.4 mmol) was stirred and heated on a 100° C. oil-bath overnight. The reaction mixture was poured into water (75 mL), and the solid was isolated by filtration, washed with water and dried. The crude product was purified by column chromatography on silica gel (Kiselgel 60, mesh 0.040-0.63) eluting with a mixture of ethyl acetate and methanol (4:1). Collecting the proper fractions afforded 600 mg (85%) of 1-[5-(4-chlorophenyl)pyridin-2-yl]-4-isopropylpiperazine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846677B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-aa31204f69794e3a9f0466e3bad627a1 |
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| 出典メモ | uspto-grants-2014_09 |
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