HuagongsheHuagongshe Chemistry Print Report · For research reference only
Difluoroacetic acid → HCID 178522122, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Difluoroacetic acid | HCID 9788 | — |
| Reactant | 2-Aminopyridine | HCID 10439 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178522122 | HCID 178522122 | 14% |
Reaction Steps
2-aminopyridine in an amount of 400 mg (4.26 mmol) was dissolved in 10 mL of anhydrous dichloromethane, following which 322 μL (490 mg, 5.11 mmol) of difluoroacetic acid, 982 mg (5.10 mmol) of EDC-HCl and 622 mg (5.11 mmol) of DMAP were added, and the mixture was stirred at room temperature for 61 hours. Following solution completion, the reaction mixture was diluted with dichloromethane, washed once with water and twice with 1% aqueous HCl, then dried over anhydrous magnesium sulfate, and concentrated under reduced pressure, giving 102 mg of 2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide (yield, 14%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09073866B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-333c9834e19d4034b30b193ace3b3854 |
| Source note | uspto-grants-2015_07 |