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Tris(2-aminoethyl)amine → 3,3,11,11-Tetramethyl-7-aminoethyl-4,7,10-triazatridecane-2,12-dione dioxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tris(2-aminoethyl)amine | HCID 77731 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Chloro-2-methyl-3-nitrosobutane | HCID 10866386 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3,3,11,11-Tetramethyl-7-aminoethyl-4,7,10-triazatridecane-2,12-dione dioxime | HCID 72359623 | 9.5% |
反応手順
To a solution of tris-(2-aminoethyl)amine (1 ml, 6.68 mmol) in acetonitrile (10 ml) was added sodium bicarbonate (1.12 g, 13.36 mmol, 2 eq). A solution of 3-chloro-3-methyl-2-nitrosobutane (1.359 g, 10.02 mmol, 1.5 eq) in dry acetonitrile (5 ml) was added slowly. The reaction mixture was left to stir at room temperature for 3 days, and then filtered. The residue was washed well with acetonitrile, and the filtrate evaporated. The crude product was then purified by RP-HPLC (System L) to afford Compound 15 (164 mg, 7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06653299B1 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-8344cf40307c48dfb48c0f21dd0d9540 |
| 出典メモ | uspto-grants-2003_11 |