Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2,2,2-Trifluoroethylamine hydrochloride | HCID 9772 | — |
| Reactant | 1-(6-Chloropyridin-3-yl)ethan-1-one | HCID 2779698 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 67509283 | HCID 67509283 | 35% |
Reaction Steps
A mixture of 1-(6-chloropyridin-3-yl)ethanone (1.0 g, 6.43 mmol) and 2,2,2-trifluoroethanamine hydrochloride (1.57 g, 11.8 mmol) in 1-methylpyrrolidin-2-one (10 mL) is stirred at 230° C. for 45 minutes under microwave irradiation. The reaction mixture is poured into water, extracted with ethyl acetate and dried over sodium sulfate and concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (4:1 to 1:1) to give 490 mg (35% yield) of the title compound as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09302991B2 |
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| Source dataset | uspto-grants-2016_04 |
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| ORD ID | ord-28ab58c62b194c9aa4bcb7b1da708d4c |
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| Source note | uspto-grants-2016_04 |
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