Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 4-Bromo-2-fluoroaniline | HCID 123050 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 2166334 | HCID 2166334 | 98.6% |
Reaction Steps
Ethyl chloroformate (15.91 g) was added dropwise to a solution of 4-bromo-2-fluoroaniline (25.33 g) and pyridine (21.06 g) in methylene chloride (260 ml) at 0° C., and the mixture was stirred at 10° C. for 3 hours. After the reaction, it was extracted with methylene chloride, then washed with diluted hydrochloric acid and an aqueous sodium hydrogencarbonate solution, and dried over anhydrous magnesium sulfate. Then, methylene chloride was distilled off, and the resulting crude crystals were crystallized from ethyl acetate-n-hexane (1:5 v/v) to obtain the objective ethyl N-(4-bromo-2-fluorophenyl)carbamate (34.45 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06174839B1 |
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| Source dataset | uspto-grants-2001_01 |
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| ORD ID | ord-6b644217c4024409ab2f48ba7aa6c90a |
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| Source note | uspto-grants-2001_01 |
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