HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 67063086, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 69038672 | HCID 69038672 | — |
| Product | HCID 67063086 | HCID 67063086 | 44% |
Reaction Steps
A mixture of 2-(5-amino-1-methyl-1 H-pyrazol-3-yl)-2-methylpropanenitrile (1.4 g, 8.5 mmol) in EtOH (30 mL) was treated with cone. H2SO4 (3 mL) and the resulting mixture was refluxed for 10 days. The reaction mixture was neutralized with saturated aq NaHCO3 solution, and the mixture was extracted with EtOAc. The organics were washed with brine, dried (MgSO4) and concentrated in vacuo. Recrystallization (EtOAc/petroleum ether) provided ethyl 2-(5-amino-1-methyl-1 H-pyrazol-3-yl)-2-methylpropanoate (0.8 g, 44% yield). 1H NMR (300 MHz, DMSO-d6): δ5.13 (s, 1 H), 5.04 (s, 2 H), 4.00 (q, J=6.9 Hz, 2 H), 3.41 (s, 3 H), 1.11 (t, J=6.9 Hz, 6 H); MS (ESI) m/z: 212.0 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08188113B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-8d8e43756bf248e9bbfbf2e308574e22 |
| Source note | uspto-grants-2012_05 |