関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Pyrimethamine | HCID 4993 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 生成物 | 2,4-Diamino-5-(3-amino-4-chloro-5-nitrophenyl)-6-ethylpyrimidine | HCID 327404 | — |
反応手順
Concentrated sulfuric acid, 90 mL, and 70% nitric acid, 90 mL, were stirred together during which time the mixture warmed to about 65° C. The mixture was allowed to cool to about 50° C., and 30.0 grams (0.12 mole) of 2,4-diamino-6-ethyl-5-(4-chlorophenyl)pyrimidine (commercially available) was added portionwise during a 45 minute period, while maintaining the reaction mixture temperature at about 50°-53° C. Upon completion of addition, the reaction mixture was stirred for one hour, while still maintaining the reaction mixture temperature at about 50° C. After this time, the reaction mixture was cooled and poured into ice. The resultant mixture was cooled further and, with stirring, was made basic with concentrated ammonium hydroxide. A precipitate was collected by filtration, rinsed with water and dried, yielding 35.4 grams of 2,4-diamino-6-ethyl-5-(4-chloro-3-nitrophenyl)pyrimidine, mp 220°-223° C., dec. The NMR spectrum was consistent with the proposed structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05521192 |
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| 出典データセット | uspto-grants-1996_05 |
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| ORD ID | ord-a354ce187e3a42f8bd87e5e13956ecee |
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| 出典メモ | uspto-grants-1996_05 |
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