HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1896022Generated: October 31, 2026
N-methyl-2-pyrrolidone → HCID 25181651, compound
https://huagongshe.com/reaction/1896022
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-Bromo-5-(trifluoromethyl)pyridine | HCID 11127991 | — |
| Reactant | 2-Methyl-6-(3-piperidin-4-ylideneprop-1-ynyl)pyridine | HCID 87550402 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 25181651 | HCID 25181651 | 1.3% |
Reaction Steps
A vial was filled with a mixture of the compound of Example 3 (84.9 mg, 0.4 mmol), 3-bromo-5-(trifluoromethyl)pyridine (93 mg, 0.4 mmol), DIPEA (140 μL, 0.8 mmol), 1 mL of anhydrous N-methylpyrrolidone and sealed. The vial was heated in a microwave oven at 160° C. (200 W) for 2 h. The reaction mixture was then cooled to r.t., diluted with EtOAc, washed with water, dried over Na2SO4 and evaporated to dryness in vacuo. The crude black oily residue was purified by preparative RP LC-MS chromatography, using MS-C18 XTerra column 30×50 mm eluting with ammonium bicarbonate 20 mM pH 8 buffer-acetonitrile gradient affording 1.8 mg of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08518916B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-6188b5095eef44d397b0d1f49dbe526d |
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| Source note | uspto-grants-2013_08 |
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