関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Bromo-2-chlorobenzoic acid | HCID 33127 | — |
| 反応物 | 3-Amino-4-nitropyridine | HCID 586943 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 66977452 | HCID 66977452 | 78.4% |
反応手順
Method C—Step a To a mixture of 5-Bromo-2-chlorobenzoic acid (5.00 g, 21.23 mmol) in DMF (40 mL), HATU (8.48 g, 22.29 mmol) and triethylamine (2.97 mL, 21.44 mmol) were added. After 30 min stirring at room temperature 4-nitro-pyridin-3ylamine (2.36 g, 16.99 mmol) was added, the reaction mixture stirred at 40° C. overnight and solvent removed. The crude was then diluted with EtOAc (40 mL) and washed first with saturated Na2CO3 solution (6×30 mL) then 1N HCl (3×30 mL). The organic layer was dried over Na2SO4, filtered and left standing. The precipitate obtained was filtered to get 4.75 g of the title compound (63%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08835648B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-8414b45ac20546a680e832ed55f2f1d1 |
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| 出典メモ | uspto-grants-2014_09 |
|---|
