関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ranisen | HCID 5039 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Zantac | HCID 47909 | — |
反応手順
Under conditions of inert atmosphere, saturated with nitrogen, suspend 10.0 g of Z, N-[2-[[[5-(dimethylamino)methyl-2-furanyl]methyl]thio]ethyl]-N′-methyl-2-nitro-1,1-ethenediamine in 100 ml of anhydrous ethyl acetate (moisture<0.01%). Add dropwise to the mixture 21.95 g of hydrochloric acid in isopropanol (concentration 5.29% mol/mol) during 45 minutes, keeping the temperature at 25° C. Stirring vigorously, again in inert nitrogen atmosphere, a white precipitate is obtained. By operating again in a nitrogen-saturated atmosphere, wash and filter the precipitate with a mixture of ethyl acetate/isopropanol in 80:20 ratio and later with ethyl acetate alone. Dry the resulting precipitate in an oven at 40°-50° C. to remove the residual solvents and afterwards place it in a drier in-vacuo on phosphorus pentoxide, until a constant weight is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06855835B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-937d0cab4258481b85f85dcdb309c617 |
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| 出典メモ | uspto-grants-2005_02 |
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