関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Bromocyclopentane | HCID 8728 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | ethyl N-(2-fluoro-4-chloro-5-methoxycarbonyloxyphenyl)carbamate | HCID 19374489 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N-[4-Chloro-5-(cyclopentyloxy)-2-fluorophenyl]carbamic acid ethyl ester | HCID 11033971 | 94.4% |
反応手順
Ethyl N-(2-fluoro-4-chloro-5-methoxycarbonyloxyphenyl)carbamate (1.45 g, 4.97 mmol) prepared by the process described in Reference Example 1 and a solution of potassium carbonate (1.03 g, 7.46 mmol) in ethanol (50 ml) were stirred for 1 hour while refluxing, and then cyclopentyl bromide (1.11 g, 7.46 mmol) was added thereto, followed by further stirring for 2 hours. After completion of the reaction, the mixture was poured into 1N hydrochloric acid (50 ml), and extracted with ethyl acetate (50 ml×3 times). The organic layer was dried, and concentrated under reduced pressure to obtain ethyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate as grey white crystals (1.41 g, 4.69 mmol, 94.4% yield). The spectral data and the like are as shown in Reference Example 1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05464811 |
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| 出典データセット | uspto-grants-1995_11 |
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| ORD ID | ord-a1eca4a2b68b45de99e271ae5f9bf604 |
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| 出典メモ | uspto-grants-1995_11 |
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