HuagongsheHuagongshe Chemistry Print Report · For research reference only
N,N-Dimethylaniline → HCID 67757094, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N,N-Dimethylaniline | HCID 949 | — |
| Reactant | 2,4-Difluorobenzoyl chloride | HCID 588081 | — |
| Reactant | HCID 19787181 | HCID 19787181 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67757094 | HCID 67757094 | 93.6% |
Reaction Steps
To a solution of 3-amino-4-(2-chlorophenyl)-6,7-dihydro-5H-cyclopenta[1',2':5,4]thieno[2,3-b]pyridine (150 mg) and N,N-dimethylaniline (0.065 ml) in dichloromethane (3 ml) was added dropwise 2,4-difluorobenzoyl chloride (0.07 ml) with ice-cooling. The mixture was stirred for 10 minutes with ice-cooling and then stirred at room temperature for 2 hours. Then, the mixture was washed in turn with water, aqueous saturated NaHCO3 solution and water, and dried over MgSO4The solvent was distilled off to obtain 4-(2-chlorophenyl)-3-(2,4-difluorobenzoylamino)-6,7 -dihydro-5H-cyclopenta[1',2':5,4]thieno[2,3-b]pyridine (206 mg, 93.6%) as crystals. The crystals were recrystallized from acetone to obtain colorless prisms, mp: 219°-220° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05143919 |
| Source dataset | uspto-grants-1992_09 |
| ORD ID | ord-87a95f813f584af59ca8c45cf45f49a0 |
| Source note | uspto-grants-1992_09 |