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Pyridine → HCID 178485978、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Quinoline | HCID 7047 | — |
| 反応物 | Diphosgene | HCID 10426 | — |
| 反応物 | 2,4-Difluorophenol | HCID 123051 | — |
| 反応物 | [4-(4-Bromo-butoxy)-cyclohexyl]-methyl-amine | HCID 22567629 | — |
| 反応物 | Sodium bicarbonate ethyl acetate | HCID 86584982 | — |
| 反応物 | HCID 178484847 | HCID 178484847 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178485978 | HCID 178485978 | — |
反応手順
A solution of 1.5 mmol trichloromethyl-chloroformate (diphosgene) in 20 ml CH2Cl2 was treated at 0° C. with 3 mmol of 2,4-difluoro-phenol and 3 mmol quinoline and then stirred for 3 h at room temperature. The reaction was then cooled (0° C.) and a solution of 1 mmol [4-(4-Bromo-butoxy)-cyclohexyl]-methyl-amine (privously prepared from trans-[4-(4-Bromo-butoxy)-cyclohexyl]-methyl-amine hydrochloride by extraction with aqueous NaHCO3/EtOAc) and 2.5 mmol pyridine in 3 ml CH2Cl2 was added. The reaction was stirred over night at room temperature, evaporated to give crude trans-[4-(4-Bromo-butoxy)-cyclohexyl]-methyl-carbamic acid 2,4-difluoro-phenyl ester which was used directly in the next step, see Example 12.39-12.44.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06858651B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-d3a966ad51af4afeb9e5f375319b6d86 |
| 出典メモ | uspto-grants-2005_02 |