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Phenyl Isothiocyanate → 2-Phenylthio-2-(3-phenyl-1,3-thiazolidine-2-yliden)acetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenyl Isothiocyanate | HCID 7673 | — |
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | (Phenylthio)acetonitrile | HCID 78891 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Phenylthio-2-(3-phenyl-1,3-thiazolidine-2-yliden)acetonitrile | HCID 4079757 | 60.1% |
反応手順
18.9 g (140 mmols) of phenylisothiocyanate and 20.9 g (140 mmols) of phenylthioacetonitrile dissolved in 50 ml of dimethylformamlde were added dropwise with stirring at room temperature to a suspension of 11.5 g of sodium hydride (60% oil, 287 mmols) in 200 ml of dimethylformamide. The mixture was stirred for 1 hour, and 28.9 g (154 mmols) of 1,2-dibromoethane was added dropwise at room temperature. Then the mixture was stirred for 3 hours. To the reaction mixture were added 300 ml of water and 100 ml of ether, followed by stirring. The precipitated crystals were collected by filtration, giving 26.1 g of the title compound as colorless crystals (yield 60%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06710062B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-a0543d76a26743c0a2a888f907e6d41f |
| 出典メモ | uspto-grants-2004_03 |