Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzonitrile | HCID 7505 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,6-Difluorobenzonitrile | HCID 74695 | — |
| Reactant | (1-Methyl-3-piperidyl)methanol | HCID 97998 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66924316 | HCID 66924316 | 4.2% |
Reaction Steps
Sodium hydride (60%; 316 mg; 7.9 mmol) was suspended in DMF and cooled to 0° C. 1-Methylpiperidin-3-ylmethanol (998 mg; 7.5 mmol) was added dropwise to the sodium hydride mixture. The solution was allowed to warm to room temperature and stirred for 30 minutes. The solution was then cooled to 0° C. 2,6-Difluorobenzonitrile (1.1 g; 7.9 mmol) in DMF was cooled to 0° C. and the alcohol mixture was added dropwise to the benzonitrile solution and allowed to warm to room temperature overnight. The solution was poured into water and extracted with dichloromethane and solvent removed. Purification by column chromatography (10% ethyl acetate/hexane) to yield 79 milligrams of 2-fluoro-6-(1-methylpiperidin-3-ylmethoxy)benzonitrile.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09067897B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-616ab713dd754c698002d50d669c63c3 |
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| Source note | uspto-grants-2015_06 |
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