HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 86732561, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | HCID 89493856 | HCID 89493856 | — |
| Catalyst | Silver trifluoroacetate | HCID 76299 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86732561 | HCID 86732561 | 99.9% |
Reaction Steps
Iodine (450 mg 1.77 mmol) was added portion wise to a solution of tert-butyl(2-{1-oxo-7-[3-(trifluoromethoxy)phenyl]-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazin-4-yl}ethyl)carbamate (780 mg 1.77 mmol) and silver trifluoroacetate (392 mg, 1.77 mmol) in dry DCM (100 ml), at 5° C. The reaction mixture was stirred at the same temperature for 1 hour, then the ice bath removed and left to warm to rt (1 h). The solid was filtered, the organic phase washed with Na2S2O5 (5% aq. solution) until decolouration occurred and finally washed with water. The organic was dried over Na2SO4 to obtain the title compound 1.0 g (99%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181258B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-429470dba2f64249ba796811a2456e8d |
| Source note | uspto-grants-2015_11 |