HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Phosphate, Tribasic → 2,6-Dichloro-5-cyclopropylnicotinonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | Tricyclohexylphosphine | HCID 75806 | — |
| Reactant | Cyclopropylboronic acid | HCID 2760897 | — |
| Reactant | 2,6-Dichloro-5-iodonicotinonitrile | HCID 84819937 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene water | HCID 22272177 | — |
| Product | 2,6-Dichloro-5-cyclopropylnicotinonitrile | HCID 84819920 | 70.3% |
Reaction Steps
A mixture of compound 2,6-dichloro-5-iodonicotinonitrile (10 g, 33.4 mmol), cyclopropylboronic acid (3.5 g, 40.1 mmol), K3PO4 (28 g, 133.6 mmol), Cy3P (1 g, 3.3 mmol) and Pd(OAc)2 (0.5 g, 2.2 mmol) in Toluene/H2O (300 mL/15 mL) was stirred under refluxing overnight. The mixture was poured into water and extracted with EtOAc. The separated organics was dried, concentrated and purified by column chromatography (Petroleum ether:EtOAc=10:1) to give compound 2,6-dichloro-5-cyclopropylnicotinonitrile (5 g, 70%). 1H-NMR (400 MHz, CDCl3) δ (ppm) 7.43 (s, 1H), 2.08 (m, 1H), 1.18 (m, 2H), 0.69 (m, 2H)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08716478B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-a725ce273e23452baf04e7fdd9b2a810 |
| Source note | uspto-grants-2014_05 |