関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloro-6-(2-Thienylmethoxy)Pyridine | HCID 18186944 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-[6-(2-Thienylmethoxy)-2-pyridinyl]piperazine | HCID 18186855 | 47% |
反応手順
A mixture of the product from step 1 above (1.35 g, 5.98 mmol), piperazine (1.55 g, 17.9 mmol) and K2CO3 (0.91 g, 6.58 mmol) in acetonitrile (5 mL) was heated at 125 125° C. for 6.5 h in a sealed pyrex flask. The reaction mixture was diluted with dichlorometane, filtered and concentrated in vacuo. The semi-solid residue was purified by silica gel (16×4 cm) chromatography using CHCl3/MeOH (9:1) as eluent. Solvents were evaporated and the oily residue was redissolved in CHCl3/ether (1:1). Filtration and concentration in vacuo furnished 0.78 g (47%) of the title compound as a beige oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07247633B2 |
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| 出典データセット | uspto-grants-2007_07 |
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| ORD ID | ord-be3db9d80a224e17b6418b7d408b3074 |
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| 出典メモ | uspto-grants-2007_07 |
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