関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Acetic acid, chloro-, pentyl ester | HCID 138488 | — |
| 反応物 | Phenol, 2-chloro-4-fluoro-5-nitro- | HCID 158655 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Chloro-2-fluoro-5-(pentyloxycarbonylmethyloxy)nitrobenzene | HCID 14617849 | 77.3% |
反応手順
A mixture of 2-chloro-4-fluoro-5-nitrophenol (100 g), anhydrous potassium carbonate (86.6 g) and dimethylformamide (500 g) was heated at 50° C., and amyl 2-chloroacetate (90.2 g) was dropwise added thereto in 30 minutes, followed by allowing to stand at 60° C. for 4 hours. The reaction mixture was cooled to room temperature, and water (1500 g) was added thereto, followed by extraction with ethyl acetate (1500 g). The organic layer was separated, washed with water and concentrated under reduced pressure. The residue was distilled under reduced pressure to give 4-chloro-2-fluoro-5-(pentyloxycarbonylmethyloxy)nitrobenzene (Compound (III)) (129 g) as a pale yellow oil. Yield, 77%. b.p., 160°-165° C./0.7 mmHg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04985570 |
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| 出典データセット | uspto-grants-1991_01 |
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| ORD ID | ord-4e61f74ca11c4edcacad9de6e4ffc51c |
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| 出典メモ | uspto-grants-1991_01 |
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