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
In 10 ml of anhydrous dichloromethane, 400 mg (4.26 mmol) of 2-aminopyridine was dissolved. To this solution, 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, followed by stirring at room temperature for 61 hours. After completion of the reaction, the reaction liquid was diluted with dichloromethane, and washed once with water, and twice with 1% HCl aq., then dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. Thus, 102 mg of 2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide was obtained (Percentage Yield: 14%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09357776B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-4866e59dc8234aacba5460889adfed29 |
| Source note | uspto-grants-2016_06 |