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2,2-Diphenylethylamine → 2-Chloro-N-(2,2-diphenylethyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,2-Diphenylethylamine | HCID 77575 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2,6-Dichloro-9-(tetrahydro-2H-pyran-2-yl)-9H-purine | HCID 270265 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 2-Chloro-N-(2,2-diphenylethyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine | HCID 10181335 | 104.1% |
反応手順
A solution of 2,6-dichloro-9-(tetrahydro-2H-pyran-2-yl)-9H-purine (Preparation 1) (30.9 g, 0.11 mol) in isopropyl alcohol (600 ml) was treated with N-ethyl-N-isopropyl-2-propanamine (47.5 ml, 0.27 mol) and 2,2-diphenylethylamine (24.8 g, 0.13 mol) and the resulting mixture heated under reflux for 3 hours. The solvent was removed under reduced pressure and the residue azeotroped with ethyl acetate. The residue was purified by column chromatography on silica gel eluting with a gradient system of ethyl acetate:hexane (40:60, by volume) gradually changing to ethyl acetate:hexane (60:40, by volume) to afford the title compound as a foam (49.7 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094769B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-403b96eddfb546f98e642649c39d1ee0 |
| 出典メモ | uspto-grants-2006_08 |