HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 20038774, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 20038761 | HCID 20038761 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 20038774 | HCID 20038774 | 90.2% |
Reaction Steps
A solution of ethyl 7-allylamino-2-(2-methoxy-2-propyl)-2H-pyrazolo[4,3-b]pyridine-6-carboxylate (2.38 g, 7.5 mmol) in dry THF (tetrahydrofuran) (25 ml) was added dropwise to an ice-cooled suspension of lithium aluminium hydride (285 mg, 7.5 mmol) in dry THF (15 ml). The mixture was stirred at room temperature, under nitrogen, for 24 h, then water (0.3 ml), 10% sodium hydroxide solution (0.3 ml) and water (0.85 ml) were added sequentially. The mixture was filtered through Kieselguhr, the solvent was evaporated in vacuo, and the residual solid was recrystallised from ethyl acetate to give the title compound as needles (1.87 g, 90%), m.p. 152°-154° C. Found: C, 60.58; H, 7.21; N, 20.26C14H20N4O2 requires C, 60.84; H, 7.29; N, 20.27%
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04837238 |
| Source dataset | uspto-grants-1989_06 |
| ORD ID | ord-4f5f5097626844d186df5bbee9b3a1fc |
| Source note | uspto-grants-1989_06 |