HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Nitrophenol → HCID 13882891, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Nitrophenol | HCID 980 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Chloro-2,6-bis-trifluoromethyl-nicotinic acid ethyl ester | HCID 13882877 | — |
| Solvent | Methyl Isobutyl Ketone | HCID 7909 | — |
| Product | HCID 13882891 | HCID 13882891 | 54.5% |
Reaction Steps
A mixture of 7.0 g (0.022 mol) of product of Example 19, 3.03 g (0.022 mol) of p-nitrophenol and 3.31 g (0.024 mol) of K2CO3 in 75 ml of methyl isobutyl ketone was refluxed for 17 hours. The cooled reaction mixture was concentrated in vacuo. The residue was dissolved in ether, washed with H2O, dried (MgSO4) and concentrated in vacuo. The residue was recrystallized in hot hexane to give 5.09 g of tan solid. The solid was purified by HPLC using 3% ethyl acetate/cyclohexane as eluting solvent affording 3.88 g (41.6%) of product as a white solid; mp 111.5°-113.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04655816 |
| Source dataset | uspto-grants-1987_04 |
| ORD ID | ord-370982278d204d4185e31ef1672a8f65 |
| Source note | uspto-grants-1987_04 |