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Dimethyl aminoterephthalate → Dimethyl 2-isocyanatoterephthalate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl aminoterephthalate | HCID 79336 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Dimethyl 2-isocyanatoterephthalate | HCID 25219824 | — |
反応手順
Dimethyl 2-aminoterephthalate (3.0 g, 14.34 mmol) and triphosgene (5.1 g, 17.22 mmol) were dissolved in toluene. Stirring was carried out at 110° C. for 6 hours under reflux to obtain 2-isocyanato-terephthalic acid dimethyl ester. After evaporating solvent, the compound was dissolved in 1,4-dioxane and triethylamine in vacuum state. After adding cyclohexylamine (2.5 mL, 21.5 mmol), stirring was carried out at 90° C. for 60 hours under reflux. After the reaction was completed, the produced solid was filtered with ether to obtain 1.75 g (37%) of 2-(3-cyclohexyl-ureido)-terephthalic acid dimethyl ester having a urea structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08748422B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-4328eab0b6a74983adbe676a9fc03334 |
| 出典メモ | uspto-grants-2014_06 |