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Sodium Carbonate → [4-({2-[(3,5-Diamino-6-chloro-pyrazine-2-carbonyl)-amino]-ethyl}-methyl-amino)-butyl]-carbamic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | tert-butyl N-(4-bromobutyl)carbamate | HCID 10868765 | — |
| 反応物 | 3,5-diamino-6-chloro-N-(2-methylaminoethyl)pyrazine-2-carboxamide | HCID 19861822 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [4-({2-[(3,5-Diamino-6-chloro-pyrazine-2-carbonyl)-amino]-ethyl}-methyl-amino)-butyl]-carbamic acid tert-butyl ester | HCID 86656659 | — |
反応手順
To a mixture comprising 3,5-diamino-6-chloro-pyrazine-2-carboxylic acid (2-methylamino-ethyl)-amide (Intermediate E) (0.5 g, 2.0 mmol) and 4-(Boc-amino)butyl bromide (0.8 g, 3.1 mmol) in DMF (5 mL) is added sodium carbonate (0.4 g, 4.0 mmol). The resulting mixture is heated at reflux for 3 h and then allowed to cool to RT, filtered and concentrated in vacuo. The crude product is dissolved in DCM and filtered to remove any undissolved impurities. The filtrate is concentrated in vacuo to yield the title compound which is used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08236808B2 |
| 出典データセット | uspto-grants-2012_08 |
| ORD ID | ord-82c095b8ca174f94b85ea27c8d891d9b |
| 出典メモ | uspto-grants-2012_08 |