HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic anhydride → HCID 57901755, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | HCID 57476167 | HCID 57476167 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 57901755 | HCID 57901755 | 92% |
Reaction Steps
To a mixture of 7-[(2-thienylsulfonyl)amino]-1H-indole-2-carboxamide (4.65 g) and pyridine (20 mL) was slowly added trifluoroacetic anhydride (4.50 mL) at 0° C., and the mixture was stirred for 1 hr. The reaction mixture was concentrated, 10% aqueous citric acid solution was added, and the resulting crystals were filtrated, washed with water and dried. The obtained crystals were subjected to silica gel column chromatography, and eluted with tetrahydrofuran-hexane (2:3, volume ratio). The eluate was treated with activated carbon and concentrated to give the title compound (4.04 g, yield 92%) as pale-yellow crystals. The crystals were recrystallized from ethyl acetate-hexane. melting point 283-284° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957070B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-cda5f657b65a4009acf0d2644afd8497 |
| Source note | uspto-grants-2015_02 |