HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic anhydride → HCID 23050245, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | HCID 23050251 | HCID 23050251 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 23050245 | HCID 23050245 | 78.2% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
5,6-Dimethoxy-benzo[b]thiophene-2-carboxamide (65 g) was suspended in pyridine (325 ml). The solution was cooled to 0° C. and treated dropwise with trifluoro acetic anhydride (185 ml) whilst maintaining the internal reaction temperature below 10° C. The mixture was then stirred at room temperature for 30 min. then cooled and treated dropwise with water (170 ml) whilst maintaining the internal temperature below 30° C. The reaction mixture was diluted with more water (800 ml), stirred and the brown solid was filtered and dried under vacuum over calcium chloride at 60° C. Recrystallisation from acetone/ether afforded 5,6-dimethoxy-benzo[b]thiophene-2-carbonitrile as a white solid (47 g), m.p. 125° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04665206 |
| Source dataset | uspto-grants-1987_05 |
| ORD ID | ord-b4c4f03adeb440378fa979d0bc7b7cae |
| Source note | uspto-grants-1987_05 |