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Sodium Carbonate → 1-[3-(Triethoxysilyl)propyl]-1,4,8,11-tetraazacyclotetradecane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1,4,8,11-Tetraazacyclotetradecane | HCID 64964 | — |
| 反応物 | (3-Iodopropyl)triethoxysilane | HCID 11782516 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-[3-(Triethoxysilyl)propyl]-1,4,8,11-tetraazacyclotetradecane | HCID 15540147 | — |
反応手順
72 g (0.359 mol) of cyclam and 15 g of Na2CO3 (dried at 100° C. under 1 mm Hg for 24 h) are placed in 2.5 l of acetonitrile in a 6 l reactor under a stream of nitrogen. The mixture is brought to reflux, a solution of 24.2 g (0.073 mol) of iodopropyltriethoxysilane in 500 ml of acetonitrile is then added dropwise and then the reaction mixture is maintained at reflux for 48 h. After evaporating the solvent on a rotary evaporator (still under a nitrogen atmosphere), pentane is added to the residue and the excess cyclam is filtered off. This operation is repeated three times, the filtrates are combined, the pentane is evaporated and compound 1 is obtained in the form of a colorless oil (15 g, 50.8%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06372903B1 |
| 出典データセット | uspto-grants-2002_04 |
| ORD ID | ord-0514501f0ef044f991efe7780a814ce4 |
| 出典メモ | uspto-grants-2002_04 |