関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Peracetic Acid | HCID 6585 | — |
| 反応物 | 2,4-Diamino-6-chloropyrimidine | HCID 67432 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | HCID 178507684 | HCID 178507684 | — |
反応手順
144.5 G. of 2,4-diamino-6-chloropyrimidine are suspended in 2000 ml. of ethanol. The suspension is warmed to 35° C. while stirring (about 15 minutes), the greater part of the material passing into solution. This mixture is then cooled down to 6°-8° C. and at this temperature there are added dropwise within 40 minutes 175 ml. of 40% peracetic acid in glacial acetic acid. After completion of the addition, the mixture is stirred at 6°-8° C. for a further 30 minutes. Thereafter, the mixture is left to warm up to room temperature, and stirred at this temperature for 3 hours. 2000 Ml. of petroleum ether are added, the mixture is stirred for 1 hour and then left to stand overnight. The separated precipitate is filtered off, back-washed with 200 ml. of petroleum ether and dried under reduced pressure, there being obtained 2,4-diamino-6-chloro-pyrimidine-3-oxide. Recrystallization yields analytically pure product having a melting point of 193° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04150131 |
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| 出典データセット | uspto-grants-1979_04 |
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| ORD ID | ord-8e32e366e0bb464a9c23ca4d3634022b |
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| 出典メモ | uspto-grants-1979_04 |
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