HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 89662143, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | HCID 89662188 | HCID 89662188 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 89662143 | HCID 89662143 | — |
Reaction Steps
1.33 g of 5-(dimethylamino)-1-(2-fluorobenzyl)-1H-pyrazole-3-carboxamide 1-10-1 (5.07 mmol, 1.0 eq.) were dissolved in 74 mL of dry THF. 1.03 mL of pyridine (12.7 mmol, 2.50 eq.) were added. Then 1.79 mL of trifluoroacetic anhydride (12.7 mmol, 2.50 eq.) were added dropwise. The reaction mixture was stirred for 24 hours at rt. Then the reaction mixture was partitioned between water and ethyl acetate. The separated aqueous layer was extracted twice with ethyl acetate. The combined organic layers were dried over sodium sulfate and concentrated in vacuo. The residue was purified by flash chromatography (hexane/ethyl acetate) to provide 406 mg (1.66 mmol, 33%) of analytically pure target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09422268B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-be4043ff013148e6a40e483089f8525f |
| Source note | uspto-grants-2016_08 |