HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Bromo-3-methylbutane → HCID 70976045, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Bromo-3-methylbutane | HCID 7891 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 70976202 | HCID 70976202 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 70976045 | HCID 70976045 | 49.1% |
Reaction Steps
To a solution of (6S,7aR)-6-Hydroxy-2-[4-(2,2,2-trifluoro-ethoxy)-phenyl]-hexahydro-pyrrolo[1,2-c]imidazol-3-one (100 mg, 0.316 mmol) in THF (3 mL) was added NaH (60% dispersion, 18.96 mg, 0.474 mmol) at room temperature and stirred for 30 min and then added 1-Bromo-3-methyl-butane (57.3 mg, 0.379 mmol) and left stirring for 12 h. The reaction mixture was quenched with NH4Cl aq., DCM was added. The organic layer was separated, washed with water and brine, dried over Na2SO4 and concentrated. The residue was purified through column chromatography (elution with ethyl acetate in hexane) to afford 60 mg (49%) of the title compound. LC-MS: 386 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08497288B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-a7a47296c58a4495a9b874f49ba3cc68 |
| Source note | uspto-grants-2013_07 |