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1,2-Dichloroethane → 4-(Cyclopentylamino)-1-ethyl-N'-isobutyryl-1H-pyrazolo[3,4-b]pyridine-5-carbohydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | 2-Methylpropanehydrazide | HCID 19239 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 4-(Cyclopentylamino)-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid | HCID 57675155 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(Cyclopentylamino)-1-ethyl-N'-isobutyryl-1H-pyrazolo[3,4-b]pyridine-5-carbohydrazide | HCID 57675192 | — |
反応手順
Intermediate 3 (0.060 g), EDC (0.06 g) and HOBT (0.035 g) were suspended in DMF (2 ml) and stirred under nitrogen for 15 minutes. Isobutyric acid hydrazide (0.027 g) was then added and the mixture stirred under nitrogen for 18 h. Solvents were removed in vacuo and the residue partitioned between DCM and water. The organic phase was washed with saturated aqueous sodium bicarbonate solution, then concentrated in vacuo and applied to an SPE cartridge (aminopropyl, 1 g) which was eluted with methanol. Concentration in vacuo afforded Intermediate 10. LCMS showed MH+=359; TRET=2.70 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07528148B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-4a9655ea6f8640b3bb2a4d9c0eecd8dc |
| 出典メモ | uspto-grants-2009_05 |