Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Bromide | HCID 6332 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Lithium | HCID 3028194 | — |
| Reactant | (2,4-Dihydroxyphenyl)(2-methoxyphenyl)methanone | HCID 12721024 | — |
| Reactant | HCID 178506846 | HCID 178506846 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57055631 | HCID 57055631 | — |
Reaction Steps
To an ethyl lithium solution prepared from 29.4 g. of ethyl bromide and 3.7 g. of lithium in 33o ml. of dry ether, under argon atmosphere, which is cooled to -10° C., a solution of 11 g. of 2-methoxy-2',4'-dihydroxy-benzophenone in 60 ml. of dry tetrahydrofurane is added dropwise, taking care that the temperature does not exceed -5° C. Thereafter the reaction mixture is stirred at 0° C. for 30 minutes and then at room temperature for two hours. The reaction mixture is decomposed with a 10% aqueous ammonium chloride solution, the phases are separated, and the aqueous phase is extracted with ether. The combined ethereal phases are washed to neutral with water, dried over anhydrous magnesium sulfate, filtered, and the solvent is distilled off in vacuo, after decoloring with activated carbon. Crystallization of the solid residue from a mixture of n-hexane and ethyl acetate yields 8.3 g. of the named compound, melting at 141° to 142° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04510338 |
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| Source dataset | uspto-grants-1985_04 |
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| ORD ID | ord-3141c4bfd75646879e603608595b5d64 |
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| Source note | uspto-grants-1985_04 |
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