関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylmorpholine | HCID 7525 | — |
| 反応物 | N-((1,1-dimethylethoxy)carbonyl)-beta-alanine | HCID 76809 | — |
| 反応物 | 2-Methylquinoline-4,6-diamine | HCID 223995 | — |
| 反応物 | O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733286 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Amino-N-(4-amino-2-methyl-quinolin-6-yl)-propionamide | HCID 17864629 | 182.5% |
反応手順
To a solution of 2.18 g (11.55 mmol) of 3-tert-Butoxycarbonylamino-propionic acid in 20 ml of DMF were added 3.78 g (11.55 mmol) TOTU. After 15 min at room temperature 2.0 g (11.55 mmol) of 2-methyl-quinoline-4,6-diamine and 2.66 g (23 mmol) of N-ethylmorpholine were added. After 24 h stirring at room temperature the solution was evaporated and the residue was treated with a saturated aqueous solution of NaHCO3. The aqueous solution was extracted with ethyl acetate. The separated organic layer was dried (Na2SO4) and evaporated. The residue was treated with 20 ml 90% trifluoroacetic acid for 2 h. After evaporation the residue was dissolve in water and extracted with ethyl acetate. The aqueous layer was lyophilized to yield 5.15 g (76%) of the title compound. MS 245.1 (M+1)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07745443B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-99c24b8d550d47829af6789f822fc3fc |
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| 出典メモ | uspto-grants-2010_06 |
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