関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cyclopentanethiol | HCID 15510 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 6-[(4-Tert-butylphenyl)(cyclopentylmethoxy)methyl]-3-chloro-2-methoxypyridine | HCID 67398052 | — |
| 生成物 | HCID 58452683 | HCID 58452683 | 25% |
反応手順
Aluminum chloride (66 mg) was added to a solution of 6-[(4-tert-butylphenyl)(cyclopentylmethoxy)methyl]-3-chloro-2-methoxypyridine (64 mg) in cyclopentanethiol (1 mL) under ice-cooling, and then the mixture was stirred at 40° C. for two hours. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and filtered, after which the solvent was evaporated under reduced pressure. The residue was purified by preparative TLC (hexane:ethyl acetate=1:10) to give the title compound as a pale yellow solid (15 mg, 25%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822503B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-647e824dcc404ac691cde1adf01144e7 |
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| 出典メモ | uspto-grants-2014_09 |
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