Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 18615632 | HCID 18615632 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 18615650 | HCID 18615650 | — |
Reaction Steps
Ethyl 4-chloro-3,6-difluoro-2-nitrophenylcarbamate (XLI) (0.9 g, 3.2 mmol) was mixed with acetic acid (30 ml) and hydrobromic acid (48%, 25 ml), the mixture was stirred at 150° C. for 4 hr and then the volume reduced to half by evaporation Ethyl acetate (50 ml) was added and the solution was washed with water (15 ml×3) and dried over sodium sulfate. The product was purified by column chromatography (silica gel, hexane) (0.56 g). 1H NMR (CDCl3, 300 MHz) 5.73 (2H, br), 7.24 (1H, dd, J=6.1, 6.1 Hz) ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | USRE039590E1 |
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| Source dataset | uspto-grants-2007_04 |
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| ORD ID | ord-2422e4a28b3645c7b67e305f206f9eb4 |
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| Source note | uspto-grants-2007_04 |
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