関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Dicyclohexylcarbamoyl chloride | HCID 222909 | — |
| 反応物 | 3-Quinolin-3-ylprop-2-yn-1-ol | HCID 650142 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 3-(3-Quinolyl)-2-Propyn-1-ol Dicyclohexyl Carbamate | HCID 11200137 | — |
反応手順
To a dry three-necked round-bottom flask equipped with nitrogen inlet and overhead stirrer was charged 3-(3-quinolyl)-2-propyn-1-ol (1 g, 5.4 mmol) in THF (10 ml) and the solution was cooled to 0° C. Potassium t-butoxide (0.67 g, 5.9 mmol) was then added followed by dicyclohexylcarbamoyl chloride (1.32 g, 5.4 mmol). The mixture was stirred for 2 hours at 0° C. and then allowed to warm up to room temperature over a period of 6 hours by which time the reaction was determined to be complete. The reaction mixture was worked up with MTBE (50 ml) and 10% NH4Cl (25 ml) and the organic layers were concentrated to an oil. The purity compared to the standard was 94% and was used as such. Yield=2 g (95%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06579986B2 |
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| 出典データセット | uspto-grants-2003_06 |
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| ORD ID | ord-d210645712bd42a79d7f4d0ab308ae3a |
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| 出典メモ | uspto-grants-2003_06 |
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