HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 86684081, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-nitro-2H-1,2,3-triazole | HCID 278150 | — |
| Reactant | Sodium chlorodifluoroacetate | HCID 2734985 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86684081 | HCID 86684081 | 48.7% |
Reaction Steps
A 100-mL single-neck round-bottomed flask containing 4-nitro-2H-1,2,3-triazole (500 mg, 4.38 mmol, 1.0 eq.), sodium 2-chloro-2,2-difluoroacetate (1310 mg, 8.76 mmol, 2.0 eq.), K2CO3 (1140 mg, 8.76 mmol, 2.0 eq.), and acetonitrile (20 mL) was stirred at reflux for 5 h. After cooling to room temperature, the reaction mixture was filtered and the filtrate was evaporated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 4:1 petroleum ether/ethyl acetate to afford 159a (350 mg, 48%) as a brown liquid. 1H NMR (500 MHz, CDCl3) δ 8.38 (s, 1H), 7.39 (t, J=57.5 Hz, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08669251B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-282ecbd0fff34a499c4f32ca8d067501 |
| Source note | uspto-grants-2014_03 |