関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Oxamic Acid | HCID 974 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | HCID 178514300 | HCID 178514300 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | HCID 178513834 | HCID 178513834 | — |
反応手順
To a mixture of 6-hydrazinyl-3-phenylpyrido[2,3-b]pyrazin-2(1H)-one (3-3) (300 mg, 1.19 mmol), HOBt (218 mg, 1.42 mmol) and oxamic acid (130 mg, 1.42 mmol) in NMP (12 mL) was added EDC (272 mg, 1.42 mmol) at room temperature and the mixture was stirred for 30 min. After addition of TFA (0.091 mL, 1.19 mmol), the mixture was heated under microwave irradiation at 150° C. for 30 minutes. To a mixture was added water (60 mL) and the precipitate was collected by filtration to give 3-hydroxy-2-phenyl[1,2,4]triazolo[4′,3′:1,6]pyrido[2,3-b]pyrazin-9-carboxamide (9-1) as a yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08207169B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
|---|
| ORD ID | ord-66a85126e86f4012a368f42eb2537669 |
|---|
| 出典メモ | uspto-grants-2012_06 |
|---|
