関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | 2-Benzenesulfonyl-5-chloropyridine | HCID 10198940 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | Phenyl 5-(1-piperazinyl)-2-pyridinyl sulfone | HCID 9839418 | 48.3% |
反応手順
To a mixture of 5-chloro-2-pyridinyl phenyl sulfone (10.2 g, 40.2 mmol) in pyridine (100 mL) was added piperazine (13.8 g, 161 mmol). The mixture was heated to 120° C. in a preheated oil bath for 18 h. The mixture then was removed from heat and cooled to room temperature. The mixture was partitioned between water and ethyl acetate. The layers were separated and the organic layer washed twice with water (2×50 mL). The organic layer was dried with anhydrous magnesium sulfate and concentrated. The solids obtained after concentration were recrystallized from water and dried to give 5.89 g of the title compound; m.p. 126-127° C.; IR (drift) 1568, 1479, 1447, 1306, 1290, 1254, 1175, 1154, 1145, 1104, 830, 756, 715, 688, 602 cm−1. 1H NMR (CDCl3) δ 3.0, 3.29, 7.13, 7.53, 8.01, 8.26.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06855709B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-8d80402db955440c94de8d01b68f81b7 |
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| 出典メモ | uspto-grants-2005_02 |
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