Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Methoxy-5-nitrophenol | HCID 69471 | — |
| Reactant | Ethane, 2-bromo-1,1-diethoxy- | HCID 74852 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 23110280 | HCID 23110280 | — |
Reaction Steps
A suspension of 7.50 g 2-methoxy-5-nitro-phenol, 9.61 g 2-bromo-1,1-diethoxy-ethane and 15.89 g cesium carbonate in 75 ml N,N-dimethylformamide was stirred at 100° C. for 4 hours. After cooling to room temperature the reaction mixture was treated with an aqueous 1% solution of sodium hydroxide and extracted twice with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate. After filtration and concentration of the solvent under reduced pressure the residue was dissolved in a mixture of ethyl acetate and n-heptane. After removal of the ethyl acetate under reduced pressure the resulting residue was filtered off and the clear solution concentrated under reduced pressure. The residue was directly subjected to the subsequent reaction without further purification. Yield: 9.45 g
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07759379B2 |
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| Source dataset | uspto-grants-2010_07 |
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| ORD ID | ord-22f040f69de640ab88cb0522b3d75a0f |
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| Source note | uspto-grants-2010_07 |
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