HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Nitrate → Methyl 4-nitro-2-(trifluoromethoxy)phenyl carbonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Nitrate | HCID 24434 | — |
| Reactant | Methyl 2-(trifluoromethoxy)phenyl carbonate | HCID 59395054 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | Methyl 4-nitro-2-(trifluoromethoxy)phenyl carbonate | HCID 59394967 | — |
| Product | Methyl 5-nitro-2-(trifluoromethoxy)phenyl carbonate | HCID 59395076 | — |
Reaction Steps
Methyl 2-(trifluoromethoxy)phenyl carbonate (200 mg, 0.85 mmol) was added portion-wise to H2SO4 (600 μL) at 0° C. to generate a colorless homogeneous solution. KNO3 (103 mg, 1.02 mmol) was added portion-wise maintaining the internal temperature below 5° C. The reaction was stirred for 2 h and then poured on ice water. The aqueous layer was extracted with dichloromethane (3×10 mL). The combined organic extracts were dried over Na2SO4, filtered and concentrated. Purification by silica gel chromatography (0-10% ethyl acetate/hexanes) provided the two regioisomers methyl 5-nitro-2-(trifluoromethoxy)phenyl carbonate (Isomer A, 120 mg) and methyl 4-nitro-2-(trifluoromethoxy)phenyl carbonate (Isomer B, 75 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367660B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-1149e6e164f9410797bf8181fff891e3 |
| Source note | uspto-grants-2013_02 |