HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 22744069, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 2-(Thiophen-3-yl)acetohydrazide | HCID 468649 | — |
| Reactant | 3-Pyridinecarboxylic acid, 4-(trifluoromethyl)- | HCID 2777549 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | HCID 22744069 | HCID 22744069 | 39.9% |
Reaction Steps
880 mg of thiophene-3-acetic hydrazide were added to a solution of 960 mg of 4-trifluoromethylpyridine-3-carboxylic acid in 5 ml of phosphorus oxychloride, and the mixture was heated at reflux for 2 hours. The reaction mixture was subsequently added dropwise to ice-water, made neutral using concentrated ammonia solution and extracted with ethyl acetate. Drying (Na2SO4), concentration and chromatographic purification gave 624 mg of the desired product as a slightly brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06239160B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-8d900bd1f9b545ec893160e6cf45cb56 |
| Source note | uspto-grants-2001_05 |