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1-Piperazinecarboxylic acid, ethyl ester → Ethyl 4-(3-hydroxypropyl)piperazine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Piperazinecarboxylic acid, ethyl ester | HCID 8431 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromo-1-propanol | HCID 12308 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Ethyl 4-(3-hydroxypropyl)piperazine-1-carboxylate | HCID 232657 | 76.3% |
反応手順
N-piperazine carboxylic acid ethyl ester (25.50 g, 161.39 mmol), 3-bromo-1-propanol (22.43 g, 161.39 mmol), potassium carbonate (55.68 g, 403.48) and anhydrous acetonitrile (200 mL) were placed in a 500 mL round bottom flask, heated for refluxing and stirred overnight. The reaction was cooled down to room temperature, filtered, concentrated and subjected to a column chromatography (eluting agent: dichloromethane/methanol/triethylamine system, v/v/v 100:1:0.5) to obtain a light yellow oily substance, 26.60 g, yield 76.3%, which was directly used in the next step of reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846678B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-85a6c53532d546d8b8522b505ecd9aa1 |
| 出典メモ | uspto-grants-2014_09 |