関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Guanidine Nitrate | HCID 10481 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloro-5-(4-nitrophenyl)-1,3,4-thiadiazole | HCID 10514277 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178512737 | HCID 178512737 | 55% |
反応手順
24.13 gm of guanidine nitrate were added in small portions over a period of 30 minutes to 6.5 gm of a 50% sodium hydride oil dispersion in 200 ml of dimethylformamide. After the evolution of hydrogen has ceased, a solution 15.8 gm of 2-chloro-5-(4-nitro-phenyl)-1,3,4-thiadiazole in 300 ml of dimethylformamide was added dropwise to the mixture, which was then stirred at room temperature for 2 hours, and then at 90° C. for 30 minutes. After cooling and dilution with water, the precipitate formed thereby was filtered off and dissolved in ethanol. Hydrogen chloride was added to this solution, and the hydrochloride which separated out was filtered off and dissolved in water, and the aqueous solution was made alkaline with 10% sodium hydroxide. The free base was filtered off, washed with water and dried, yielding 9.5 gm of the title compound, m.p. 295°-297° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04645841 |
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| 出典データセット | uspto-grants-1987_02 |
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| ORD ID | ord-b1130618595f4ea0bf6f0c74b22af9cf |
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| 出典メモ | uspto-grants-1987_02 |
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