関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 反応物 | 2-(2-Methylthioethoxy)aniline | HCID 54213163 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(2-Methylthioethoxy)-phenylhydrazine | HCID 54289290 | — |
反応手順
27.4 g of the aniline obtained under (b) are placed into 45 ml of glacial acetic acid and, with ice cooling, a mixture of 37 ml of concentrated HCl and 75 ml of H2O is added. The formed suspension is diazotised at 0°-5° C. with 10.3 g of NaNO2 in 22 ml of water. The diazonium solution is subsequently stirred at 0° C. for 10 minutes, and a solution of 80.7 g of SnCl2.2H2O in 112 ml of concentrated HCl is then quickly added with cooling. After 4 hours, water is added to the reaction mixture, and extraction is repeatedly performed with ether. The aqueous phase is afterwards rendered alkaline with a 10% aqueous sodium hydroxide solution, and extracted three times with ether. After customary further processing of the ether phases, there is obtained the compound of the formula ##STR61## having a melting point of 72.5°-74.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04725302 |
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| 出典データセット | uspto-grants-1988_02 |
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| ORD ID | ord-8ff8d568cf1248518f7da91bcabe7759 |
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| 出典メモ | uspto-grants-1988_02 |
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