Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | 2-Dimethylaminopyridine | HCID 21885 | — |
| Reactant | 2-Amino-5-chlorobenzonitrile | HCID 80019 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 14810936 | HCID 14810936 | — |
Reaction Steps
(Step 1) To a solution of 2-amino-5-chlorobenzonitrile (1.95 g) and dimethylaminopyridine (20.3 mg) in N,N-dimethylacetamide (15 ml) was added dropwise methyl chlorocarbonate (3.5 ml) at room temperature, and the mixture was stirred at 90° C. for 5 hr. The mixture was allowed to cool to room temperature, poured into water, and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and filtered. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=3:20-1:4) to give methyl (4-chloro-2-cyanophenyl)carbamate (1.21 g) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07982044B2 |
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| Source dataset | uspto-grants-2011_07 |
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| ORD ID | ord-4328808e363c40c987ae14bd6fe51158 |
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| Source note | uspto-grants-2011_07 |
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