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p-Toluenesulfonic acid → 6-chloro-8-(2,5-dimethoxybenzyl)-N9-butyl purine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | N-(4-butylamino-6-chloro-pyrimidin-5-yl)-2-(2,5-dimethoxyphenyl)acetamide | HCID 11660875 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 6-chloro-8-(2,5-dimethoxybenzyl)-N9-butyl purine | HCID 85827657 | — |
反応手順
A mixture of N-(4-butylamino-6-chloro-pyrimidin-5-yl)-2-(2,5-dimethoxyphenyl) acetamide (1 mmol) and p-TSA (0.5 mmol) in toluene was refluxed for 72 h. Solvent was removed, diluted with EtOAc and washed with water, bicarbonate and dried. Purification on a silica gel column (200-400 mesh, Fisher Scientific, Tustin, Calif., USA) gave 6-chloro-8-(2,5-dimethoxybenzyl)-N9-butyl purine. Rf=0.65 in 1:1 EtOAc:hexane. 1H NMR (DMSO-d6) δ 8.7 (s, 1H), 6.96 (d, 1H), 6.84 (m, 1H), 6.8 (dd, 1H), 4.28 (s, 2H), 4.23 (t, 2H), 3.69 (s, 3H), 3.67 (s, 3H), 1.62 (m, 2H), 1.25 (m, 2H), 0.88 (t, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07241890B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-867b123fb1914c5d8e5db6b8d90fc0cb |
| 出典メモ | uspto-grants-2007_07 |