HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Sulfate → HCID 69058379, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 86635792 | HCID 86635792 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69058379 | HCID 69058379 | 69.8% |
Reaction Steps
To a stirred suspension of lithium aluminum hydride (400 mg) in THF (25 ml) was added a solution of ethyl(2-amino-5-bromo-3-methylphenyl)carbamate (1 g) in THF (10 ml) at 0° C. The mixture was then warmed to room temperature, followed by heating at reflux for 1 h. The reaction mixture was cooled to 0° C., diluted with THF (45 ml) and a saturated Na2SO4 solution was added dropwise thereto. The mixture was further stirred for 30 min and solids were filtered over Celite. The filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/EtOAc) to give the title compound (550 mg) as a brownish liquid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09365540B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-a2f615fbf76447cea15cecd4fbdea3a6 |
| Source note | uspto-grants-2016_06 |