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Ethylamine → 3-Chloro-2-fluorobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylamine | HCID 6341 | — |
| 反応物 | 3-Chloro-2-fluoro-6-(trimethylsilyl)benzoic acid | HCID 18630211 | — |
| 生成物 | 3-Chloro-2-fluorobenzoic acid | HCID 302931 | 84% |
| 生成物 | 3-Chloro-N-ethyl-2-fluoro-6-(trimethylsilyl)benzamide | HCID 18630098 | — |
反応手順
The trimethylsilyl ester of 3-chloro-2-fluorobenzoic acid (11.66 g) was prepared in 84% yield using the method described in Example 207. This ester (2.47 g) was converted to 0.45 g of 3-chloro-2-fluoro-6-(trimethylsilyl)benzoic acid in 18% yield using the method of Example 207. The crude product was converted to the acid chloride by the procedure of example b. The acid chloride was reacted with 70% aq ethylamine using General Method El to afford the title compound. Purification by flash chromatography (ethyl acetate/hexanes) followed by recrystallization from pentane gave 84 mg of the title compound as an off-white solid (18%). m.p. 96-97° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06028101 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-d0fd0d20c582432b87fddefefe2ff44c |
| 出典メモ | uspto-grants-2000_02 |