HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → Ethyl 2-ethoxy-4-fluoro-5-nitrobenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Potassium Nitrate | HCID 24434 | — |
| Reactant | Ethyl 2-ethoxy-4-fluorobenzoate | HCID 59198761 | — |
| Product | Ethyl 2-ethoxy-4-fluoro-5-nitrobenzoate | HCID 59198570 | — |
Reaction Steps
In nitrogen atmosphere, to ethyl 2-ethoxy-4-fluorobenzoate as synthesized in above Production Example 31, 6.51 g, conc. sulfuric acid 34 mL was added under cooling with ice. Potassium nitrate 3.26 g was further added little by little, under cooling with salt-ice, followed by stirring for 3.4 hours under cooling with ice. The reaction liquid was poured in ice water, and the precipitated crystals were recovered by filtration and washed with water. Recrystallizing the crystals from tert-butyl methyl ether-hexane mixed solvent, 4.49 g of the title compound was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040536B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-c82d091b05e445afa83fcb9ee8f50234 |
| Source note | uspto-grants-2015_05 |