HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Dimethylaminopyridine → HCID 9865190, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Dimethylaminopyridine | HCID 21885 | — |
| Reactant | N,N-Dimethylethylenediamine | HCID 66053 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | PyBroP | HCID 2733179 | — |
| Reactant | HCID 18542421 | HCID 18542421 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 9865190 | HCID 9865190 | — |
Reaction Steps
A mixture of 3-[2-(3,4-difluorophenylamino)acetylamino]-2-methylbenzoic acid (0.2 g), N,N-dimethylethylenediamine (0.08 ml), bromotripyrrolidinophosphonium hexafluorophosphate (PyBroP®) (0.34 g), dimethylaminopyridine (0.07 g) and N,N-diisopropylethylamine (0.31 ml) in dimethylformamide (5 ml) was stirred at room temperature under N2 for 18 hours. The reaction mixture was partitioned between ethyl acetate and water and the organic phase was washed with water and brine, dried (MgSO4) and evaporated. The crude product was triturated with diethyl ether. The resultant solid was triturated with ethyl acetate and filtered. Yield 70 mg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06555541B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-478e01b551bc4070ab84ee3a6110e5f5 |
| Source note | uspto-grants-2003_04 |