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2,3,6-Trichlorobenzoic acid → (Aminocarbonyl)Methyl 2,3,6-Trichlorobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,3,6-Trichlorobenzoic acid | HCID 5759 | — |
| 反応物 | Chloroacetamide | HCID 6580 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (Aminocarbonyl)Methyl 2,3,6-Trichlorobenzoate | HCID 2417794 | — |
反応手順
This compound was prepared in the manner of Example I, using 15.0 grams (0.066 mole) of 2,3,6-trichlorobenzoic acid, 4.4 grams (0.066 mole) of potassium hydroxide, 6.2 grams (0.066 mole) of 2-chloroacetamide, and 1.8 grams of 1,4,7,10,13,16-hexaoxacyclooctadecane in 300 ml of dry toluene and 200 ml of dimethylformamide. The crude product was purified by liquid chromatography, followed by recrystallization from ethyl acetate. The yield was 0.9 gram of (aminocarbonyl)methyl 2,3,6-trichlorobenzoate; mp 158°-160°. The ir and the nmr spectra were consistent with the proposed structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04309566 |
| 出典データセット | uspto-grants-1982_01 |
| ORD ID | ord-f67ddac55063423aa6c6229eb1daa2d8 |
| 出典メモ | uspto-grants-1982_01 |