関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylenediamine | HCID 3301 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Propanoic acid, 2-bromo-2-methyl-, ethyl ester | HCID 11745 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Piperazinone, 3,3-dimethyl- | HCID 211157 | 68.8% |
反応手順
A solution of ethyl-2-bromoisobutyrate (24 mL, 161 mmol) in toluene (150 mL) was added to a mixture of ethylene diamine (70 mL, 1046 mmol, 6.5 equiv) and potassium carbonate (24.4 g, 177 mmol, 1.1 equiv) in toluene (150 mL). The reaction mixture was heated for 20 h at 115° C., cooled and filtered. The filtrate was concentrated and the residue triturated in Et2O to afford 14.2 g of the title compound as a yellow solid: ESI-MS: 129.1 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08536175B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-b6f1359851554a6e8633af1cffc9717a |
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| 出典メモ | uspto-grants-2013_09 |
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