Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | 3,5-Difluorophenylacetic acid | HCID 145424 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | HCID 53879162 | HCID 53879162 | — |
Reaction Steps
A solution of 3,5-difluorophenylacetic acid (20 g, Fluorochem) in c.H2SO4 (150 ml) was stirred at -15° C. and c.HNO3 (75 ml) added dropwise over 1 hour at a temperature of from -5° to -10° C. The mixture was stirred for a further 1/2 hour at -10° C. and then poured into ice-water (1.0 l). The latter was extracted with ether (×3) and the combined extracts washed with water (×2), dried over MgSO4, and evaporated under reduced pressure to give a solid which was crystallised and then recrystallised from ether/hexane (1:4 v/v) to give 20.8 g of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05290814 |
|---|
| Source dataset | uspto-grants-1994_03 |
|---|
| ORD ID | ord-7f90211a5ebe4998b5bf2f962de450a2 |
|---|
| Source note | uspto-grants-1994_03 |
|---|