HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1,1-Trifluoro-2-propanol → 4-(2,2,2-Trifluoro-1-methylethoxy)pyridine-2-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1,1-Trifluoro-2-propanol | HCID 9774 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 4-Chloro-2-pyridinecarbonitrile | HCID 693342 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-(2,2,2-Trifluoro-1-methylethoxy)pyridine-2-carbonitrile | HCID 59570382 | 78.5% |
Reaction Steps
Into 6 ml of N,N-dimethylformamide was suspended 0.16 g of sodium hydride (60% oily), and 0.4 g of 1,1,1-trifluoro-2-propanol was added at 10° C. After stirring for 40 minutes, 0.4 g of 4-chloropyridine-2-carbonitrile was added, the mixture was stirred for 2 hours, and the reaction solution was poured into an aqueous saturated ammonium chloride solution, followed by extraction with tert-butyl=methyl=ether three times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.49 g of 4-(2,2,2-trifluoro-1-methylethoxy)pyridine-2-carbonitrile.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08318776B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-6c518184814d4e21a6fd7d8396e86788 |
| Source note | uspto-grants-2012_11 |