HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 4-(4-Methoxyphenyl)-3-nitropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | (4-Methoxyphenyl)boronic acid | HCID 201262 | — |
| Reactant | 4-Chloro-3-nitropyridine hydrochloride | HCID 12244206 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | 4-(4-Methoxyphenyl)-3-nitropyridine | HCID 15366418 | — |
Reaction Steps
4-Methoxyphenylboronic acid (24.54 g), 4-chloro-3-nitropyridine hydrochloride (26.24 g), Pd(Ph3P)4 (4 g) and K2CO3 (111 g) were combined in DME (500 mL). The reaction was heated to reflux for 10 hours. After the mixture cooled down to room temperature, it was poured into saturated aqueous NH4OAc (500 mL) solution. The aqueous phase was extracted with EtOAc (3×200 mL). The combined extract was concentrated to give a residue which was purified using silica gel chromatography (10% to 30% EtOAc/PE) to afford 10.6 g of Precursor 1, 3-Nitro-4-(4-methoxyphenyl)pyridine. MS m/z: (M+H)+ calcd for C12H11N2O3: 231.08; found 231.02. HPLC retention time: 1.07 minutes (column B).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07662823B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-fb6bf9b09e054517b3282472e683340b |
| Source note | uspto-grants-2010_02 |