Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 3,4,5-Trifluoro-N-methyl-2-nitrobenzenamine | HCID 71300096 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 86762004 | HCID 86762004 | — |
Reaction Steps
A solution of methyl(3,4,5-trifluoro-2-nitrophenyl)amine (0.5 g) in acetic acid (7.5 ml) is treated portionwise with zinc powder (793 mg). The reaction medium is stirred at ambient temperature (20° C.) until complete reduction. Water (13 ml) and 28% ammonia are added to pH 7, and then the reaction medium is depleted using ethyl acetate (3×50). The organic extracts are combined, dried over magnesium sulphate, filtered and evaporated under reduced pressure. The oil obtained is taken up in ether (50 ml) and then 2N HCl is added thereto. The solid formed is filtered off. 3,4,5-Trifluoro-N1-methylbenzene-1,2-diamine is isolated in its hydrochloride form (508 mg), and is used in the next stage.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08507483B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-179b571865224c29a6b734a7ce70ba58 |
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| Source note | uspto-grants-2013_08 |
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