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Methanol → 9-Ethyl-3-isocyanatocarbazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Amino-9-ethylcarbazole | HCID 8588 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 溶媒 | Carbon Disulfide | HCID 6348 | — |
| 生成物 | 9-Ethyl-3-isocyanatocarbazole | HCID 20155099 | — |
反応手順
38.6 g of 3-amino-9-ethylcarbazole and 27.9 ml of triethylamine were added to 300 ml of methanol, and, while cooling with ice, 15.2 g of carbon disulfide was added dropwise thereto. After conducting reaction at room temperature for 3 hours, 41.3 g of dicyclohexylcarbodiimide was added thereto, followed by reacting at room temperature for 4 hours. Crystals thus precipitated were collected by filtration, heat-refluxed for 10 minutes in 500 ml of ethyl acetate, and cooled to precipitate and then filter off solids. The filtrate was concentrated by removing solvents in vacuo to obtain the desired product (29 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04607006 |
| 出典データセット | uspto-grants-1986_08 |
| ORD ID | ord-9eba8f1869a947b2b8374ea56de86b98 |
| 出典メモ | uspto-grants-1986_08 |