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Benzylamine → 2-[4-(3-Bromo-4-methoxy-phenoxy)-3,5-dimethyl-phenyl]-3,5-dioxo-2,3,4,5-tetrahydro-[1,2,4]triazine-6-carboxylic acid benzylamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| 反応物 | 2-[4-(3-Bromo-4-methoxy-phenoxy)-3,5-dimethyl-phenyl]-3,5-dioxo-2,3,4,5-tetrahydro-[1,2,4]triazine-6-carboxylic acid | HCID 22339438 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dce dmf | HCID 20184825 | — |
| 生成物 | 2-[4-(3-Bromo-4-methoxy-phenoxy)-3,5-dimethyl-phenyl]-3,5-dioxo-2,3,4,5-tetrahydro-[1,2,4]triazine-6-carboxylic acid benzylamide | HCID 69707610 | — |
反応手順
To a solution of benzylamine (6 μmol) in 10% DMF/DCE were added sequentially 10% DMF/DCE solutions of 2-[4-(3-bromo-4-methoxy-phenoxy)-3,5-dimethyl-phenyl]-3,5-dioxo-2,3,4,5-tetrahydro-[1,2,4]triazine-6-carboxylic acid (5 μmol) and N-methylmorpholine (6 μmol). A DMF solution of O-benzotriazol-1-yl-N,N,N′,N′-tetramethyluronium hexafluorophosphate (7.5 μmol) and the resulting solution was shaken for 4 h at room temperature. The reaction was concentrated at 60° C. in a vacuum oven overnight. HPLC and LCMS shows complete conversion to the title compound of Step A. MS Calc.: 550.1; Found: 549.0 (M−1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06930107B2 |
| 出典データセット | uspto-grants-2005_08 |
| ORD ID | ord-3a0cd9f79afc4c75bdb22e24d633d67f |
| 出典メモ | uspto-grants-2005_08 |