HuagongsheHuagongshe Chemistry Print Report · For research reference only
t-Butyl 3-(4-bromophenyl)-1-(methoxy(methyl)amino)-1-oxopropan-2-ylcarbamate → t-Butyl 1-(4-bromophenyl)-3-oxohexan-2-ylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | t-Butyl 3-(4-bromophenyl)-1-(methoxy(methyl)amino)-1-oxopropan-2-ylcarbamate | HCID 18779134 | — |
| Reactant | HCID 178455851 | HCID 178455851 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | t-Butyl 1-(4-bromophenyl)-3-oxohexan-2-ylcarbamate | HCID 66863791 | 56.9% |
Reaction Steps
A solution of propylmagnesium bromide (29.7 g, 201.6 mmol, 3.0 equiv) in THF (200 mL) was added dropwise with stirring at 0° C. to a solution of the carbamate (26 g, 66.5 mmol, 1.0 equiv) in THF (200 mL). The resulting solution was stirred overnight at room temperature. The reaction was then quenched by the addition of aqueous NH4Cl (200 mL). The resulting solution was extracted with EtOAc and the organic layers combined. The resulting mixture was washed with saturated NaHCO3 (200 mL) and saturated aqueous NaCl (200 mL), then dried over anhydrous MgSO4. The residue was applied onto a silica gel column with petroleum ether/EtOAc (5:1) to yield t-butyl 1-(4-bromophenyl)-3-oxohexan-2-ylcarbamate (14 g) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181206B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-8a74778347054a6cb65034e4a68a45d3 |
| Source note | uspto-grants-2015_11 |