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Cesium carbonate → [5-(2,2-Dimethyl-3-oxo-piperazin-1-ylmethyl)-pyridin-2-yl]-carbamic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-Piperazinone, 3,3-dimethyl- | HCID 211157 | — |
| 反応物 | tert-Butyl (5-(bromomethyl)pyridin-2-yl)carbamate | HCID 23030321 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [5-(2,2-Dimethyl-3-oxo-piperazin-1-ylmethyl)-pyridin-2-yl]-carbamic acid tert-butyl ester | HCID 66914612 | 67.7% |
反応手順
A mixture of intermediate 100.2 (Step 100.2) (18.4 g, 64 mmol), 3,3-dimethyl-piperazin-2-one (Step 108.4) (9 g, 70 mmol, 1.1 equiv) and Cs2CO3 (27.1 g, 83.2 mmol, 1.3 equiv) in DMF (75 ml) was stirred for 12 h at rt, quenched by addition of H2O (500 mL) and filtered to afford 14.5 g of the title compound as an off-white solid. Title compound: ESI-MS: 335.2 [M+H]+; tR=2.22 min (System 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536175B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-365abdac828c4d17b2f502cb950ced9a |
| 出典メモ | uspto-grants-2013_09 |