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N-(2,6-dichloropyrimidin-4-yl)acetamide → N-{2-Chloro-6-[1-(3-ethoxy-4-methoxy-benzyl)-piperidin-4-ylamino]-pyrimidin-4-yl}-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-(2,6-dichloropyrimidin-4-yl)acetamide | HCID 4713752 | — |
| 反応物 | 1-(3-Ethoxy-4-methoxy-benzyl)-piperidin-4-ylamine | HCID 39257445 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | N-{2-Chloro-6-[1-(3-ethoxy-4-methoxy-benzyl)-piperidin-4-ylamino]-pyrimidin-4-yl}-acetamide | HCID 86618534 | 3% |
反応手順
A solution of N-(2,6-dichloro-pyrimidin-4-yl)-acetamide (30.9 mg, 0.15 mmol, 1.0 equiv) and 1-(3-ethoxy-4-methoxy-benzyl)-piperidin-4-ylamine (47.6 mg, 0.18 mmol, 1.2 equiv; intermediate A1) in DMAc (2 mL) was heated by microwave irradiation to 180° C. for 15 min. Removal of the solvent under reduced pressure and purification by preparative HPLC on reversed phase eluting with a gradient of acetonitrile/water provided 1.6 mg (3%) of the title compound. MS (ISP): 434.4 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07968568B2 |
| 出典データセット | uspto-grants-2011_06 |
| ORD ID | ord-7a741dd6a00a4ce3bcc0392de29e799b |
| 出典メモ | uspto-grants-2011_06 |