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Triethylamine → [1-[[(1H-Benzimidazol-2-ylmethyl)amino]carbonyl]-2-methylbutyl]carbamic acid 1,1-dimethylethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzimidazol-2-ylmethylamine dihydrochloride hydrate | HCID 145819 | — |
| 反応物 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 反応物 | tert-Butoxycarbonyl-L-isoleucine | HCID 2724762 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | [1-[[(1H-Benzimidazol-2-ylmethyl)amino]carbonyl]-2-methylbutyl]carbamic acid 1,1-dimethylethyl ester | HCID 67747066 | 88.4% |
反応手順
To a room temperature solution of 0.505 g N-(tert-butoxycarbonyl)-L-isoleucine in 10 ml of methylene chloride is added, in the following order, 0.50 g of 2-(aminomethyl)benzimidazole dihydrochloride hydrate, 1.07 g of BOP and 0.850 g of triethylamine. The reaction is stirred at room temperature for 2 hours, diluted with methylene chloride, and washed with saturated sodium chloride. The organic layer is dried, filtered, and concentrated in vacuo. Purification by chromatography (silica gel; 70% ethyl acetate/hexane) gives 0.669 g of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05428167 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-b2ebf4b4fc064d1fb082620a179a8a10 |
| 出典メモ | uspto-grants-1995_06 |