Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 54276775 | HCID 54276775 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 15906595 | HCID 15906595 | — |
Reaction Steps
2.06 g (0.0106×1.2 mol) of 3-(trifluoromethyl) phenol was dissolved in about 20 ml of DMF. The solution was further mixed with 0.45 g (ca. 60% in mineral oil; 0.0106×1.06 mol) of NaH and then with 3.00 g (0.0106 mol) of 2,6-dibromo-4-methylmercapto pyridine. After stirring at about 110° C. for about 2 hours, the mixture was allowed to stand for cooling to room temperature. After the reaction solution was distributed in hexane-saturated sodium bicarbonate water, the organic phase of the obtained solution was washed with saturated brine and dried with anhydrous sodium sulfate. The resultant solution was concentrated and then purified by silica gel column chromatography (eluting solution: ethyl acetate/hexane), and the obtained eluate was subjected to recrystallization using hexane, thereby obtaining an aimed product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06339045B1 |
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| Source dataset | uspto-grants-2002_01 |
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| ORD ID | ord-fe460f794bfe4fe88382f1046a7fa93f |
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| Source note | uspto-grants-2002_01 |
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