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Diisopropylethylamine → 4-(1-((2-chloro-9-methyl-6-morpholino-9H-purin-8-yl)methyl)piperidin-4-yl)morpholine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-Morpholinopiperidine | HCID 795724 | — |
| 反応物 | 4-(8-(bromomethyl)-2-chloro-9-methyl-9H-purin-6-yl)morpholine | HCID 59603481 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(1-((2-chloro-9-methyl-6-morpholino-9H-purin-8-yl)methyl)piperidin-4-yl)morpholine | HCID 59603495 | 95% |
反応手順
To a solution of 4-(8-(bromomethyl)-2-chloro-9-methyl-9H-purin-6-yl)morpholine (935 mg, 2.7 mmol) in DCM (30 mL) was added 4-morpholino-piperidine (505 mg, 2.97 mmol) and DIEA (0.70 mL). The resulting mixture was stirred at room temperature for 18 hours. The mixture was then poured onto water and the layers were separated. The aqueous layer was extracted with three times with DCM. The combined organic extracts were washed with water, dried over Na2SO4, filtered and concentrated. The crude product was then purified by flash chromatography (0-30% gradient MeOH in DCM) to give the title compound as a white solid (95%). LCMS: M+H+=436.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08158625B2 |
| 出典データセット | uspto-grants-2012_04 |
| ORD ID | ord-b862ae862dcf45b299df1ab5a96cd78c |
| 出典メモ | uspto-grants-2012_04 |