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1-(3-Aminopropyl)-4-methylpiperazine → (2-{2-[3-(4-Methylpiperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophen-6-ylmethyl)-carbamic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(3-Aminopropyl)-4-methylpiperazine | HCID 78328 | — |
| 反応物 | [2-(2-Chloropyrimidin-4-yl)-benzo[b]thiophen-6-ylmethyl]-carbamic acid tert-butyl ester | HCID 86625348 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (2-{2-[3-(4-Methylpiperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophen-6-ylmethyl)-carbamic acid tert-butyl ester | HCID 68859103 | 70.2% |
反応手順
A mixture of [2-(2-chloropyrimidin-4-yl)-benzo[b]thiophen-6-ylmethyl]-carbamic acid tert-butyl ester (1.47 g, 3.90 mmol) and 1-(3-aminopropyl)-4-methylpiperazine (1.36 g, 8.60 mmol) in dioxane (38 mL) is refluxed for 3 hours. The solvent is removed and the residue is subjected to chromatography on silica gel, eluting with 2.0 M NH3/MeOH in CHCl3 0-10%, to obtain the title compound (1.36 g, 70% yield). ES+(m/z) 497 [M+H].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07547691B2 |
| 出典データセット | uspto-grants-2009_06 |
| ORD ID | ord-09c30005acbf4e2d84c146f67df2fb9b |
| 出典メモ | uspto-grants-2009_06 |