HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 559816Generated: October 31, 2026
Calcium Carbonate → HCID 66725396, compound
https://huagongshe.com/reaction/559816
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Calcium Carbonate | HCID 10112 | — |
| Reactant | 2-Butanone, 3-bromo- | HCID 13142 | — |
| Reactant | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Reactant | HCID 66725294 | HCID 66725294 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 66725396 | HCID 66725396 | 13% |
Reaction Steps
6-Methyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2-dihydro-pyridine-3,5-dicarboxylic acid 5-amide 4-methanesulfonyl-benzylamide (see Example 60, 0.05 g, 0.098 mmol), 3-bromo-2-butanone (0.020 g, 0.20 mmol), CaCO3 (0.015 g, 0.15 mmol), NMP (1.5 ml) and a magnetic stirrer bar were placed in a tube designed for microwave synthesis. The vial was sealed and the mixture was heated in a CEM Discover Microwave apparatus (100 W, 140 ° C.) for 2 h. The reaction was stopped and the crude mixture was dissolved in acetonitrile (2 ml) and water (2 ml) and was purified directly on preparative HPLC, giving the title compound (0.007 g, 13%) as a slightly brownish solid after freeze-drying the pure fractions.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08063073B2 |
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| Source dataset | uspto-grants-2011_11 |
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| ORD ID | ord-d40241082a9e44bfa8d546c278cd5551 |
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| Source note | uspto-grants-2011_11 |
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