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Ammonium Chloride → 3-Chloro-4-[4-(2,4-dichlorobenzylidene)cyclohexyl]amino-2-ethylpyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-(2,4-Dichlorobenzylidene)cyclohexylamine | HCID 19694016 | — |
| 反応物 | 3,4-Dichloro-2-ethylpyridine | HCID 21708425 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 3-Chloro-4-[4-(2,4-dichlorobenzylidene)cyclohexyl]amino-2-ethylpyridine | HCID 19694009 | 7% |
反応手順
1.6 g of 3,4-dichloro-2-ethylpyridine and 2.5 g of 4-(2,4-dichlorobenzylidene)cyclohexylamine are heated at 180° C. for 3.5 hours together with 55 g of ammonium chloride in 9 ml of N-methylpyrrolidone. After cooling, the mixture is poured into saturated sodium bicarbonate solution and extracted with ethyl acetate. The product is purified by chromatography on silica gel using ethyl acetate/heptane 1:4. Yield: 7%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723450 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-c0062b7363ec4154b00b2b22681d2f1d |
| 出典メモ | uspto-grants-1998_03 |