HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 3-Thiophenecarboxamide,N-ethyl-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Thiophene-3-carboxylic acid | HCID 6918 | — |
| Reactant | Ethylamine hydrochloride | HCID 11198 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-Thiophenecarboxamide,N-ethyl- | HCID 15452328 | 76% |
Reaction Steps
A mixture of 3-thiophenecarboxylic acid (20 g, 178 mmol), thionyl chloride (30 mL), and DMF (5 drops) was stirred overnight, then was concentrated under vacuum and stripped several times from toluene to remove all traces of excess thionyl chloride. Pyridine (31.64 g, 400 mmol) was added dropwise to a mixture of this acid chloride and ethylamine hydrochloride in toluene (5 mL) and CH2Cl2 (50 mL). After stirring for 1 h, the reaction was washed with 10% aq HCl followed with water, then was dried (MgSO4), concentrated, and crystallized from ethyl acetate/hexanes to give 14.9 g of N-ethyl-3-thiophenecarboxamide as a tan solid, a 76% yield. m.p. 115°-117° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05811411 |
| Source dataset | uspto-grants-1998_09 |
| ORD ID | ord-e52985957dfa4ac6a37ce6c698b33d55 |
| Source note | uspto-grants-1998_09 |