化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 4-(4-Imino-2-thioxo-1-(4-methylphenyl)-1,3-diazaspiro[4.5]dec-3-yl)-2-trifluoromethylbenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Isothiocyanato-2-(trifluoromethyl)benzonitrile | HCID 11615540 | — |
| 反応物 | Propan-2-one--dichloromethane (1/1) | HCID 21584124 | — |
| 反応物 | 1-p-Tolylaminocyclohexanecarbonitrile | HCID 59839099 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(4-Imino-2-thioxo-1-(4-methylphenyl)-1,3-diazaspiro[4.5]dec-3-yl)-2-trifluoromethylbenzonitrile | HCID 86609854 | 8% |
反応手順
Triethylamine (0.05 g, 0.5 mmol) was added to a solution of 1a (0.228 g, 1 mmol) and 9a (0.214 g, 1 mmol) in dry THF (2 ml). The reaction mixture was stirred at room temperature for 2 days and then concentrated to yield a dark residue which was subjected to flash chromatography (dichloromethane/acetone, 95:5) to afford 4-(4-imino-2-thioxo-1-(4-methylphenyl)-1,3-diazaspiro[4.5]dec-3-yl)-2-trifluoromethylbenzonitrile, 9b (0.035 g, 0.08 mmol, 8%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08658681B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-502f5d41c4a84ab9a2d22f622a5107c6 |
| 出典メモ | uspto-grants-2014_02 |