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1,3-Propanediamine → Benzyl (3-aminopropyl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Propanediamine | HCID 428 | — |
| 反応物 | Benzyl phenyl carbonate | HCID 11183772 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Benzyl (3-aminopropyl)carbamate | HCID 417669 | — |
反応手順
To a solution of 1,3-propanediamine (6.50 g, 87.0 mol) in 250 mL of abs. EtOH was added benzyl phenyl carbonate (20.0 g, 87.0 mmol). The solution was stirred overnight. A white precipitate formed. The solvent was removed in a rotary evaporator, and the residue was taken up with 100 ml of distilled H2O. This was followed by acidification with 2M HCl to pH 1-2, and 4× extracting with 250 mL of CH2Cl2 each time. The aqueous phase was rendered strongly alkaline with 2M NaOH and extracted 4× with 250 mL of CH2Cl2 each time. The combined organic phases were dried over Na2SO4, subsequently the solvent was removed in a rotary evaporator to obtain the product as a viscid white mass (4.70 g, 26%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08865863B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-5405fbd92faa4027a0d90af56d769c72 |
| 出典メモ | uspto-grants-2014_10 |