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Triethylamine → HCID 90006117、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,4,7,10-Tetraazacyclododecane | HCID 64963 | — |
| 反応物 | 2-Chloro-N-(phenanthridin-6-ylmethyl)acetamide | HCID 86712484 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 90006117 | HCID 90006117 | 47.1% |
反応手順
A solution of the chloro 9 (20.0 mg, 70.2 μmol) in anhydrous CHCl3 (5 mL) was added to a solution of cyclen (48.4 mg, 0.281 mmol) and triethylamine (11.7 μL, 84.2 μmol) in anhydrous CHCl3 (15 mL) under N2 (g). The reaction mixture was heated to reflux under N2 (g) for 23 hours. The reaction mixture was then allowed to cool to room temperature and washed with NaOH (aq) (1.0 M, 3×5 mL) and H2O (3×5 mL). The organic phase was dried over MgSO4, and concentrated under reduced pressure yielding product 10 as a colorless oil (13.9 mg, 47.1%). This procedure follows closely that developed by Gunnlaugsson and coworkers. (Massue et al. Tetrahedron Lett., 2007, 48, 8052-8055).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09194802B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-7032c9cfaf014cd299a8313934d2b44b |
| 出典メモ | uspto-grants-2015_11 |