HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22078400, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | 2-amino-3-fluorophenol | HCID 2782778 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22078400 | HCID 22078400 | — |
Reaction Steps
To a mixture of 2-amino-3-fluorophenol (2.07 g) and dichloromethane (100 mL) were added TEA (2.29 mL) and methyl chloroformate (1.27 mL) under ice-cooling, followed by stirring at room temperature for 3 hours. The reaction mixture was ice-cooled, and 0.5 M hydrochloric acid solution was added thereto, followed by stirring for 10 minutes. Then, the organic layer was separated. The organic layer was washed with brine, dried over Na2SO4, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: Hex/EtOAc=100/0-75/25) to obtain methyl (2-fluoro-6-hydroxyphenyl)carbamate (2.55 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08937087B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-1787a579f2fd4bd8a97b9a8e3b2956a7 |
| Source note | uspto-grants-2015_01 |