HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Propanol → HCID 66959030, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Propanol | HCID 1031 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-(tert-Butylcarbonylamino)phenylboronic acid | HCID 4193502 | — |
| Reactant | HCID 66958775 | HCID 66958775 | — |
| Catalyst | Triphenylphosphine | HCID 11776 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 66959030 | HCID 66959030 | 40.4% |
Reaction Steps
4-Bromo-5-butyl-1-tert-butyl-1H-pyrazole-3-carbonitrile (3.0 g, 10.6 mmol) was treated with triphenylphosphine (0.085 g, 0.32 mmol), 2-[(2,2-dimethylpropanoyl)amino]phenylboronic acid (prepared as described in Part G of Example 23, 2.41 g, 15.8 mmol), 1-propanol (22 mL), palladium (II) acetate (0.024 g, 0.11 mmol), 2 M aqueous sodium carbonate (6.5 mL, 13.0 mmol), and water (4.4 mL) according to the general procedure described in Examples 37-39. The crude product was purified by chromatography on a HORIZON HPFC system (silica gel, gradient elution with 0-25% ethyl acetate in hexanes) to yield 1.63 g of N-[2-(5-butyl-1-tert-butyl-3-cyano-1H-pyrazol-4-yl)phenyl]-2,2-dimethylpropanamide as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09145410B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-663ee9d3e78843c8a1b363497ad107e1 |
| Source note | uspto-grants-2015_09 |