HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 15231616, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 3-tert-butyloxycarbonylamino-4-(2-methylphenyl)-7,8-dihydro-6H-cyclopenta[g][1]benzopyran-2-one | HCID 19782166 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15231616 | HCID 15231616 | 98.4% |
Reaction Steps
To a solution of 3-tert-butyloxycarbonylamino-4-(2methylphenyl) -7,8-dihydro-6H-cyclopenta [g] [1 ]benzopyran-2-one (2.05 g) in dichloromethane (20 ml) was added trifluoroacetic acid (10 ml) dropwise with ice-cooling. The mixture was stirred under ice-cooling for 1 hour, after which the solvent was distilled off. The residue was diluted with water, neutralized with saturated aqueous solution of NaHCO3 and extracted with chloroform. The extract was washed with water and dried (MgSO4) and the solvent was distilled off to give crystals of 3-amino-4-(2-methylphenyl)-7,8-dihydro-6H-cyclopenta[g] [1]-benzopyran-2-one (1.5 g, 98.4%). Recrystallization from ethanol-dichloromethane gave colorless prisms, m.p. 275°-276° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05418239 |
| Source dataset | uspto-grants-1995_05 |
| ORD ID | ord-ef64be96741b445a80d575ce071b802a |
| Source note | uspto-grants-1995_05 |