HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-(5-Amino-3-tert-butyl-pyrazol-1-yl)-propan-1-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pentanenitrile, 4,4-dimethyl-3-oxo- | HCID 108871 | — |
| Reactant | 3-Hydrazinylpropan-1-ol dihydrochloride | HCID 50988434 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 3-(5-Amino-3-tert-butyl-pyrazol-1-yl)-propan-1-ol | HCID 86686731 | 85.4% |
Reaction Steps
A solution of 4,4-dimethyl-3-oxo-pentanenitrile (0.7 g, 5.58 mmol) in ethanol (IMS grade, 5 mL) was treated with 3-hydrazino-propan-1-ol dihydrochloride (1 g, 6.13 mmol), followed by cone. HCl (0.05 mL), and the reaction mixture was heated at reflux for 18 h. The mixture was concentrated in vacuo and the residue was purified by FCC, using 0-10% [2M NH3 in MeOH] in DCM to afford the title compound as a white gummy solid (0.94 g, 85%). LCMS (Method 3): Rt 0.42 min, m/z 198 [MH+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835431B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-98787d0f6a47411b9a18f0a0e6f2a14c |
| Source note | uspto-grants-2014_09 |