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Ethyl bromoacetate → Ethyl (1,4,8,11-tetraazacyclotetradec-1-yl)ethanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,4,8,11-Tetraazacyclotetradecane | HCID 64964 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Ethyl (1,4,8,11-tetraazacyclotetradec-1-yl)ethanoate | HCID 12963737 | — |
反応手順
In a first phase, ethyl (1,4,8,11-tetraazacyclotetradec-1-yl)ethanoate is obtained by slowly adding 6.68 g (40.0 mmol) of ethyl bromoacetate onto a solution of 40 g (200.0 mmol) of cyclam and 16 g (116 mmol) of potassium carbonate in 1 L of chloroform. The reaction mixture is maintained under stirring at room temperature for 48 h. After filtration on celite and evaporation of the solvent, the residue is taken up in petroleum ether. The excess cyclam is filtered off, the filtrate is concentrated and ethyl (1,4,8,11-tetraazacyclotetradec-1-yl)ethanoate (so-called compound 5.0) is thereby obtained, as 11.21 g of a slightly yellow oil (yield=98%) which is used without any purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08975395B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-e3de51cb07fe422a8eb5cc6ed19af054 |
| 出典メモ | uspto-grants-2015_03 |