関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Butanol | HCID 263 | — |
| 反応物 | Butylamine | HCID 8007 | — |
| 反応物 | 2-Chloroadenine | HCID 94904 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | HCID 178448875 | HCID 178448875 | 83% |
反応手順
2-chloroadenine (1) (1.60 g, 9.44 mmol) was divided among three microwave vials (10-20 mL), each containing Butylamine (4 mL), 1-Butanol (10 mL,), and DMSO (1 mL). Each vial was heated to 170° C. for 90 minutes. After reaction completion the solvent was removed by rotary evaporation and the product was purified on flash column eluting 10% methanol in ethylacetate. Evaporation of solvent gave 1.62 g (83%) of 64 as an off white solid. 1H NMR (300 MHz, DMSO) δ 0.877 (t, 3H), 1.29 (m, 2H), 1.45 (m, 2H), 3.17 (t, 2H), 6.49 (s, 2H), 7.61 (s, 1H), 12.1 (s, 1H). LCMS: m/z for C9H14N6++H observed 207.2 at 1.40 minutes of a 3.5 minute run, gradient 5-95% CH3CN in H2O.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08338593B2 |
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| 出典データセット | uspto-grants-2012_12 |
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| ORD ID | ord-e2b86ccd86d34646be0b9cf1d8fe480b |
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| 出典メモ | uspto-grants-2012_12 |
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