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Tetrahydrofuran → 8-(4-Iodo-2-methoxy-pyridin-3-yl)-6-methyl-2-morpholin-4-yl-9H-purine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Iodo benzene diacetate | HCID 12217721 | — |
| 反応物 | N5-(4-Iodo-2-methoxy-pyridin-3-ylmethylene)-6-methyl-2-morpholin-4-yl-pyrimidine-4,5-diamine | HCID 58819980 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 8-(4-Iodo-2-methoxy-pyridin-3-yl)-6-methyl-2-morpholin-4-yl-9H-purine | HCID 178494186 | 36% |
反応手順
To a solution of N5-(4-Iodo-2-methoxy-pyridin-3ylmethylene)-6-methyl-2-morpholin-4-yl-pyrimidine-4,5-diamine (140 mg, 0.31 mmol) in a mixture of MeOH:THF (20 mL: 10 mL) was added iodobenzene diacetate (198 mg, 0.62 mmol). After stirring at ambient temperature for 4 hours, the solvents were evaporated in vacuo and the crude was purified by preparative HPLC (see method below) to give the title compound as an amber solid (50 mg, 36%): IR (KBr, cm−1) 3420, 2853, 1618; 1H NMR (400 MHz, CDCl3) δ 9.63 (s, 1H), 7.83 and 7.54 (d, J=5.3, 1H), 3.91 (s, 3H), 3.81–3.77 (m, 8H), 2.72 (s, 3H); LCMS (+ESI, M+H+) m/z 453; HPLC: 97% (220 nm).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07189716B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-3f6a966281734c0e8afd9d502cafa527 |
| 出典メモ | uspto-grants-2007_03 |