Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 4-Aminophenol | HCID 403 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 54909083 | HCID 54909083 | — |
Reaction Steps
To a solution of sodium hydroxide (730 mg, 18.25 mmol) in methanol was added 4-aminophenol (2.00 g, 18.32 mmol). After the resulting mixture was made to dissolve, methanol was evaporated under reduced pressure. To the residue was added DMF (20 mL), and then 2-chloro-5-nitropyridine (2.91 g, 18.35 mmol). The reaction solution was stirred for 1.5 hours at 70° C., and then concentrated under reduced pressure. Water was added to the residue, and the resulting solution was extracted with ethyl acetate. The ethyl acetate layer was washed with brine. The ethyl acetate layer was dried over anhydrous magnesium sulfate, after which solvent was evaporated, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1), to thereby yield 3.37 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08236826B2 |
|---|
| Source dataset | uspto-grants-2012_08 |
|---|
| ORD ID | ord-f24e8689427d4b9aa2c90ec4622a8b70 |
|---|
| Source note | uspto-grants-2012_08 |
|---|