関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 6-Chloro-N4-(4-chlorophenyl)pyrimidine-4,5-diamine | HCID 16726311 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | N4-(4-chlorophenyl)6-pyrrolidin-1-yl-pyrimidine-4,5-diamine | HCID 21905785 | — |
反応手順
6-Chloro-N4-(4-chlorophenyl)-pyrimidine-4,5-diamine I-(1A-1)a (114 mg, 0.45 mmol) and pyrrolidine (1 ml, excess) were combined and heated with stirring at 100° C. for 2 hours. The reaction mixture was diluted with saturated NaHCO3 solution and extracted with ethyl acetate. The organic layers were combined, dried (Na2SO4), filtered, and evaporated to dryness to yield the desired compound I-(17A-1)a (131 mg, quantitative) as an orange-brown solid: +ESI MS (M+1) 290.3; 1H NMR (500 MHz, CD3OD) δ 7.85 (s, 1H), 7.45 (d, J=8.8 Hz, 2H), 7.26 (d, J=8.8 Hz, 2H), 3.63 (m, 4H), 1.96 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07129239B2 |
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| 出典データセット | uspto-grants-2006_10 |
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| ORD ID | ord-71d7bad0cd694211a11f6ce4945b6b59 |
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| 出典メモ | uspto-grants-2006_10 |
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