関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chlorobenzoxazole | HCID 11986 | — |
| 反応物 | Ethyl 4-amino-5-chloro-2-fluorophenylacetate | HCID 17858807 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Ethyl (4-(2-benzoxazolyl)amino-5-chloro-2-fluorophenyl)acetate | HCID 58778947 | 74% |
反応手順
In xylene (4 ml), 2-chlorobenzoxazole (278 μl, 2.43 mmol) and ethyl (4-amino-5-chloro-2-fluorophenyl)acetate (512 mg, 2.21 mmol) were heated under reflux for 2 hours. After the reaction mixture was cooled to room temperature, the solvent was distilled off under reduced pressure. The residue was dissolved in ethyl acetate. The resulting solution was washed with a saturated aqueous solution of sodium bicarbonate, dried over anhydrous sodium sulfate, and distilled under reduced pressure to remove the solvent. The residue was purified by chromatography on a silica gel column, whereby from n-hexane/ethyl acetate (7:1, v/v) eluate fractions, ethyl (4-(2-benzoxazolyl)amino-5-chloro-2-fluorophenyl)acetate (570 mg, 74%) was obtained as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07157487B2 |
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| 出典データセット | uspto-grants-2007_01 |
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| ORD ID | ord-4f7bd92e4e4c47be9740591b36e80cac |
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| 出典メモ | uspto-grants-2007_01 |
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