関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chlorobenzaldehyde | HCID 6996 | — |
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | 2-Thiopheneethylamine, hydrochloride | HCID 458572 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | [2-(2-Thienyl)ethylamino](2-chlorophenyl)acetonitrile | HCID 10858772 | — |
反応手順
9.8 g (0.2 mol) of sodium cyanide is dissolved in 70 ml of water and to the solution first 32.8 g (0.2 mol) of 2-(2-thienyl)ethylamine hydrochloride, then in a period of a few minutes, the solution of 28.2 g (0.2 mol) of o-chlorobenzaldehyde in 30 ml of ethanol are added. During the addition the temperature of the mixture raises to 45° C. The reaction mixture is then stirred at 60° C. for 2 hours, then cooled to room temperature and diluted with 50 ml of water. The resulting oily product is extracted with 100 ml of 1,2-dichloroethane, the organic phase is washed to cyanide-free with 2×50 ml of water, the traces of 2-(2-thienyl)ethylamine are removed by treatment with 20 ml of 3% hydrochloric acid solution. The residual fast crystallizing oil is the product. Weight: 52 g (94%) mp.: 40-41° C. The product was identified as written in Example 1. Quality of the product is identical with that of the product prepared according to Example 1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06215005B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-62cf43c0690c4f35bf3045ac534888d7 |
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| 出典メモ | uspto-grants-2001_04 |
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