関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 2-Methylquinoline-4,6-diamine | HCID 223995 | — |
| 反応物 | N-(4-amino-2-methyl-6-quinolyl)-2-amino-4,6-dichloro-5-methylsulfanylpyrimidine | HCID 22250299 | — |
| 生成物 | N,N'-bis(4-amino-2-methyl-6-quinolyl)-2,4-diamino-6-chloro-5-methylsulfanyl-pyrimidine | HCID 69588754 | — |
反応手順
A mixture of 43 mg of N-(4-amino-2-methyl-6-quinolyl)-2-amino-4,6-dichloro-5-methylsulfanylpyrimidine and 55 mg of 4,6-diamino-2-methylquinoline in 5 mL of ethanol is heated under reflux for about 3 hours, left at a temperature in the region of 20° C. for about 16 hours and then filtered. The filtrate is concentrated under reduced pressure (2.7 kPa) at a temperature in the region of 40° C., and then the residue obtained is purified by HPLC (column: C18 Waters, 5 M, 50×19 mm; eluent: elution gradient water-acetonitrile-TFA (0.07%) from 95-5 to 5-95 over 30 minutes). The fractions containing the desired product are combined and concentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the region of 40° C. to obtain 12 mg of N,N′-bis(4-amino-2-methyl-6-quinolyl)-2,4-diamino-6-chloro-5-methylsulfanyl-pyrimidine in the form of a beige colored solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06995175B2 |
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| 出典データセット | uspto-grants-2006_02 |
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| ORD ID | ord-9bf56a2bfb094f739b344600036807a4 |
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| 出典メモ | uspto-grants-2006_02 |
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