関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Naphthoic acid | HCID 6847 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 4,5-Pyrimidinediamine, 6-chloro- | HCID 78010 | — |
| 生成物 | HCID 178478392 | HCID 178478392 | 80.4% |
反応手順
A mixture of 6-chloro-4,5-diaminopyrimidine (519 mg, 0.00359 mol) and 1-naphthalenecarboxylic acid (618 mg, 0.00359 mol) in phosphoryl chloride (2.0 mL, 0.021 mol) was heated at 110° C. under an atmosphere of nitrogen for 5.5 hours. The reaction was cooled and the residue was washed several times with ether. The residue was dissolved in CH2Cl2 and aqueous NaHCO3. The layers were separated and the aqueous was extracted with EtOAc (1×) and CH2Cl2 (1×). The combined organics were washed with saturated aqueous NaHCO3, brine, dried (Na2SO4), filtered, and collected in vacuo to obtain 810 mg (80%) of an orange solid. LC/MS: Rt=1.68 min, ES+ 261 (FA standard).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08481550B2 |
|---|
| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-41a32a5df1bb4cad9563b4deb9aae78d |
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| 出典メモ | uspto-grants-2013_07 |
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