Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | 2-Methylpyridine | HCID 7975 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Bromo-2'-nitroacetophenone | HCID 244025 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 118970840 | HCID 118970840 | — |
Reaction Steps
First, 4.1 mmol of 2-bromo-2′-nitroacetophenone and 5.33 mmol (1.3 eq.) of picoline are dissolved into 12 ml of acetone and the reaction mixture is allowed to react at 90° C. for 3 hours. After the completion of the reaction, the reaction mixture is cooled at room temperature and filtered, and then the filtered solid is washed with 5 ml of dichloromethane. To 20 ml of acetonitrile, 4.1 mmol of the obtained solid and 20.5 mmol (5 eq.) of triethylamine are added. Then, the reaction mixture is allowed to react at 60° C. for 16 hours. After the completion of the reaction, the reaction mixture is concentrated under reduced pressure, and then the concentrated reaction mixture is purified by silica gel column chromatography using hexane:ethyl acetate:dichloromethane=30:1:2 as a solvent to obtain the target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09296751B1 |
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| Source dataset | uspto-grants-2016_03 |
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| ORD ID | ord-1a1346afa93341bf9cfa083c333b5b24 |
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| Source note | uspto-grants-2016_03 |
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