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Fmoc isothiocyanate → N-(4-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl)-N'-(fluoren-9-ylmethyloxycarbonyl)thiourea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Fmoc isothiocyanate | HCID 4154759 | — |
| 反応物 | 6-Aminomethyl-4-ethoxy-N-methylnicotinamide | HCID 57791297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | N-(4-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl)-N'-(fluoren-9-ylmethyloxycarbonyl)thiourea | HCID 57791308 | 74.6% |
反応手順
500 mg (2.39 mmol) of 6-aminomethyl-4-ethoxy-N-methylnicotinamide (Example 12f) were dissolved in 25 ml of dioxane and treated at RT with 672.4 mg (2.39 mmol) of fluoren-9-ylmethyloxycarbonyl isothiocyanate. After one hour, the mixture was freed from the solvent and the residue was taken up in DCM. It was washed three times with aqueous LiCl solution and once with water. After drying with MgSO4, the mixture was concentrated and the crude product (875 mg) thus obtained was reacted further without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863269B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-2629fc5befd24b84a8d127c603379184 |
| 出典メモ | uspto-grants-2011_01 |