HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → HCID 58911537, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 11176570 | HCID 11176570 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | HCID 58911537 | HCID 58911537 | 25.5% |
Reaction Steps
A solution of (R)-8 trifluoromethyl-1,2,3,4,11,11a-hexahydro-pyrazino[1,2-b]isoquinolin-6-one (245 mg, 0.9 mmol) in H2SO4 (2 mL) was treated with NBS (210 mg, 1.17 mmol) at room temperature. After 48 h, the reaction mixture was quenched with saturated aqueous NaHCO3 and diluted with EtOAc (15 mL). The solution was extracted with EtOAc (50 mL) and the organic layer was dried over Na2SO4, filtered, and concentrated in vacuo to afford a yellow oil. Purification of the oil by flash column chromatography (SiO2, 96:4:1 methylene chloride/methanol/triethylamine) provided (R)-10-bromo-8-trifluoromethyl-1,2,3,4,11,11a-hexahydropyrazino[1,2-b]isoquinolin-6-one (80 mg, 25%) as an off-white solid. MS (ESI) 349 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07244843B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-f81bf85e85964b87896ad3bed764fc82 |
| Source note | uspto-grants-2007_07 |