化工社化工社 化学情報印刷レポート · 研究参考用
1-Bromooctadecane → 10-Octadecyl-1,4,7,10-tetraazacyclododecane-1,4,7-triacetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Bromooctadecane | HCID 8218 | — |
| 反応物 | Tri-tert-butyl 1,4,7,10-Tetraazacyclododecane-1,4,7-triacetate | HCID 11237632 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 10-Octadecyl-1,4,7,10-tetraazacyclododecane-1,4,7-triacetic acid | HCID 9962140 | — |
反応手順
A mixture of 1,4,7,10-tetraazacyclododecane-1,4,7-triacetic acid tris(1,1-dimethylethyl)ester (37.5 g; 72.8 mmol) and 1-bromooctadecane (24.5 g; 73.5 mmol) in CH3CN (500 mL) was heated to reflux. After 2 h the reaction mixture was evaporated and the residue was dissolved in CHCl3 and a portion of CF3COOH was added. After 16 h at room temperature the reaction mixture was evaporated and the oily residue dissolved in CF3COOH. After 3 days at room temperature, the solution was evaporated, the residue taken up in CHCl3 and the solution evaporated. This operation was repeated three times. The oily residue was purified by flash chromatography as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06652834B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-a664bd2018a943e3a5baf1503454e641 |
| 出典メモ | uspto-grants-2003_11 |