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5,5-Dimethyl-2,4-imidazolidinedithione → 2,4-bis(2-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5,5-Dimethyl-2,4-imidazolidinedithione | HCID 3002142 | — |
| 反応物 | 2-(chloromethyl)-N,N-dimethylaniline hydrochloride | HCID 13537426 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2,4-bis(2-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole | HCID 18934848 | — |
反応手順
Initially, a solution of 9.1 g of 2-dimethylaminobenzylchloride hydrochloride in 50 mL of EtOH was added to a solution of 7 g of 5,5-dimethyl-2,4-dithiohydantoin in 100 mL of ethanol (EtOH). The reaction mixture was stirred for 1.5 hour at the room temperature and concentrated in vacuo. To the residue, there was added 100 mL of chloroform (CHCl3). The residue was then washed with an aqueous solution of potassium carbonate (CaCO3), dried over magnesium sulfate (MgSO4), and concentrated in vacuo. The residue was chromatographed on a column of silica gel (CHCl3). From the earlier fractions, 2,4-bis(2-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole was isolated as a syrup. The yield of this compound was 1.1 g with a yield ratio of 5.9%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05733922 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-a4c2572338d149fc9b4505fc6cb945cf |
| 出典メモ | uspto-grants-1998_03 |