HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 60755716, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | Benzenamine, 3-bromo-4-methyl- | HCID 82187 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 60755716 | HCID 60755716 | 90.1% |
Reaction Steps
Methyl chloroformate (0.202 ml, 2.62 mmol) was added to a solution of 3-bromo-4-methyl-phenylamine (243 mg, 1.31 mmol) in pyridine (2 ml), and the mixture was stirred at room temperature overnight. H2O was added to the reaction mixture, followed by extraction with AcOEt (×2). The organic layers were combined and sequentially washed with H2O and saturated brine, and then dried over Na2SO4 and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (n-hexane/AcOEt) to give (3-bromo-4-methyl-phenyl)-carbamic acid methyl ester (288 mg, 90%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169254B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-02777fb17c8c42489e34d370a2029d50 |
| Source note | uspto-grants-2015_10 |