HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 67091069, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | o-Tolylhydrazinium(1+) chloride | HCID 71554 | — |
| Reactant | Pentanenitrile, 4,4-dimethyl-3-oxo- | HCID 108871 | — |
| Product | HCID 67091069 | HCID 67091069 | 92% |
Reaction Steps
A solution of tolyl hydrazine hydrochloride (8.0 g, 50 mmol) and 4,4-dimethyl-3-oxo-pentanenitrile (6.3 g, 50 mmol) in toluene (30 mL) was heated to reflux overnight. Removal of the volatiles in vacuo provided a residue, which was purified by silica gel chromatography using 30% ethyl acetate in hexanes as the eluent. Concentration in vacuo provided 3-amino-5-tert-butyl-2-tolyl-2H-pyrazole as a brown solid (10.5 g, 92%). LC-MS analysis of the compound indicates the desired product is present with a purity >99%. Calculated mass=229. Observed mass=230.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07897599B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-bc71adf8a5034db9b5a7ded118c19f43 |
| Source note | uspto-grants-2011_03 |