참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Peracetic Acid | HCID 6585 | — |
| 반응물 | 2,4-Diamino-6-chloropyrimidine | HCID 67432 | — |
| 용매 | Acetic acid 10-acetoxymethyl-anthracen-9-ylmethyl ester | HCID 613145 | — |
| 생성물 | HCID 178507684 | HCID 178507684 | — |
반응 단계
144.5 G. of 2,4-diamino-6-chloropyrimidine are suspended in 2000 ml. of ethanol. While stirring, the suspension is warmed to 35° C. (about 15 minutes), the greater part of the substance passing into solution. The mixture is then cooled to 6°-8° C. and, at this temperature, there are added dropwise within the course of 40 minutes 175 ml. of 40% peracetic acid in glacial acetic. After completion of the addition, the mixture is stirred at 6°-8° C. for a further 30 minutes. The mixture is then left to warm up to room temperature and stirred at this temperature for 3 hours. 2000 Ml. of petroleum ether are then added, the mixture is left to stir 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-chloropyrimidine-3-oxide. Recrystallization yields analytically pure product, having a melting point of 193° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04175189 |
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| 출처 데이터셋 | uspto-grants-1979_11 |
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| ORD ID | ord-40bc849c5eb9465eb24eb84deec4062d |
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| 출처 메모 | uspto-grants-1979_11 |
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