Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | Trifluoromethanesulfonic acid | HCID 62406 | — |
| Reactant | HCID 22920243 | HCID 22920243 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22919105 | HCID 22919105 | 89.9% |
Reaction Steps
In a 1-liter three-necked flask equipped with a stirring device, a thermometer and a nitrogen substituting device, 32.6 g of 1,2-bis(4-(4-nitrobenzoyl)phenyl)ethane and 200 milliliters of dichloromethane were introduced. 42.0 g of trifluoromethane sulfonic acid was added dropwise for 15 minutes. Subsequently, a solution of 40.7 g of triethylsilane in 50 milliliters of dichloromethane was added dropwise for 1 hour. After the end of the dropwise addition, stirring was carried out for 18 hours with warming to room temperature. After the end of the reaction was confirmed by a liquid chromatography, the reaction solution was neutralized with an aqueous solution of sodium carbonate and washed with water. After removing dichloromethane by a rotary evaporator, 27.6 g of 1,2-bis(4-(4-nitrobenzyl)phenyl)ethane was obtained as crystals by recrystallizing from a toluene solvent.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05663440 |
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| Source dataset | uspto-grants-1997_09 |
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| ORD ID | ord-c09c5530a4ff48e18063d6e4ec734eec |
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| Source note | uspto-grants-1997_09 |
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