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Hydrochloric Acid → methyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate
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 | methyl N-(2-fluoro-4-chloro-5-hydroxyphenyl)carbamate | HCID 19042327 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | methyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate | HCID 15766845 | 84.8% |
反応手順
Cyclopentyl bromide (4.07 g, 27.3 mmol) was added to an acetonitrile solution (50 ml) containing methyl N-(2-fluoro-4-chloro-5-hydroxyphenyl)carbamate (5.00 g, 22,8 mmol) and potassium carbonate (1.80 g, 13.0 mmol), and the mixture was heated under reflux for 4 hours. After reaction, the reaction liquid was cooled to room temperature, 1N hydrochloric acid (50 ml) was added thereto, and this was extracted with ethyl acetate (50 ml×2). The organic layer was washed with water and then dried over anhydrous magnesium sulfate. The drying agent was removed by filtration, and the solvent was removed by distillation under reduced pressure to obtain methyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate (5.56 g, 19.3 mmol). Yield: 84.8%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05391807 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-3756c97c09dc4e36832c364b3c3517c9 |
| 出典メモ | uspto-grants-1995_02 |