Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Stannous chloride dihydrate | HCID 61436 | — |
| Reactant | 3-(1,1-Dimethylethyl)-6-nitro-5-(trifluoromethyl)-1H-indole | HCID 68462630 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67261454 | HCID 67261454 | — |
Reaction Steps
A microwave vial charged with 3-tert-butyl-6-nitro-5-(trifluoromethyl)-1H-indole (95 mg, 0.3319 mmol), SnCl2.2H2O (375 mg, 1.66 mmol) and ethanol (1 mL), was sealed and heated at 62° C. for 3 h. The reaction was cooled to room temperature, diluted with EtOAc and quenched with saturated NaHCO3 solution until the pH was 7. The reaction mixture was then filtered through a plug of celite. The layers were separated and the organic layer was dried over Na2SO4, filtered and concentrated. The residue was purified via silica gel column chromatography using 0 to 40% EtOAc in hexanes to obtain 3-tert-butyl-5-(trifluoromethyl)-1H-indol-6-amine. LC/MS: m/z 257.3 (M+H)+ at 1.54 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08802700B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-c3c7fc0f502a467b88e4ca335c306738 |
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| Source note | uspto-grants-2014_08 |
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