Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | HCID 10521771 | HCID 10521771 | — |
| Reactant | 4'-(Trifluoromethyl)-[1,1'-biphenyl]-2-carbonyl chloride | HCID 11066000 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86754924 | HCID 86754924 | 97% |
Reaction Steps
The title product of Example 3 (0.38 g, 1.1 mmol) and triethylamine (0.17 mL, 1.2 mmol) were dissolved in methylene chloride (14 mL) and stirred at room temperature while a solution of 4'-trifluoromethylbiphenyl-2-carbonyl chloride (0.31 g, 1.1 mmol) in methylene chloride (40 mL) was added dropwise. After four hours, 10% aq sodium carbonate solution was added and the mixture was stirred for thirty minutes. The methylene chloride layer was washed with brine, dried over magnesium sulfate and evaporated in vacuo to afford the title product as a hard foam, 0.63 g, 97% yield. 1H NMR (CDCl3) δ 7.79 (s, 1), 7.72 (d, 1), 7.64 (d, 2), 7.58-7.34 (m, 6), 7.12 (d, 2), 7.01 (s, 1), 6.90-6.72 (m, 4), 5.38 (s, 2), 3.73 (s, 3), 3.69 (s, 2), 3.50 (s, 2), 2.79 (t, 2), 2.68 (t, 2). IR (KBr) 1668, 1615, 1599, 1567, 1536, 1514 cm-1. Mass spectrum: m/z: 598 (M+ -1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05998623 |
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| Source dataset | uspto-grants-1999_12 |
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| ORD ID | ord-4a0f7116041b4d0bbb6bdc5a2f6f2d48 |
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| Source note | uspto-grants-1999_12 |
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