関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | N-BOC-ethylenediamine | HCID 187201 | — |
| 反応物 | (2-Bromoethyl)tritylamine | HCID 15718287 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Tert-butyl 2-{[2-(tritylamino)ethyl]amino}ethylcarbamate | HCID 18442413 | 41.8% |
反応手順
To a solution of tert-butyl 2-aminoethylcarbamate (4.81 g) in dehydrated chloroform (10 ml) were added sodium carbonate (1.06 g) and N-(2-bromoethyl)tritylamine (3.66 g), and the mixture was stirred under reflux for 3 hours. To the reaction mixture were added diethyl ether and hexane, and the solution was washed with water. The mixture was extracted with 5% aqueous citric acid solution, and the aqueous layer was washed with diethyl ether. The aqueous layer was then made alkaline with sodium hydrogencarbonate followed by extraction with diethyl ether. The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to give tert-butyl 2-{[2-(tritylamino)ethyl]amino}ethylcarbamate (1.86 g) as a viscous oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07192943B2 |
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| 出典データセット | uspto-grants-2007_03 |
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| ORD ID | ord-f7d27343a9094619b1ae392f183741ec |
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| 出典メモ | uspto-grants-2007_03 |
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