Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Morpholine | HCID 8083 | — |
| Edukt | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| Edukt | 2-Bromo-4-iodoanisole | HCID 3376779 | — |
| Edukt | Sodium t-butoxide | HCID 23676156 | — |
| Katalysator | palladium(II) acetate | HCID 167845 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 67429791 | HCID 67429791 | — |
Reaktionsschritte
Under nitrogen atmosphere, to a solution of 20.0 g of 2-bromo-4-iodoanisole in toluene (250 ml) was added morpholine (6.12 ml), 1.29 g of tri-tert-butyl phosphine, 13.5 g of sodium tert-butoxide, and 359 mg of palladium acetate (II), and the reaction mixture was stirred for two hours at 45° C. Water and EtOAc were added to the reaction solution, liquid separation was performed and the aqueous layer was extracted with EtOAc. The combined organic layer was washed with saturated brine, dried over MgSO4, then, the drying agent was separated by filtration, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by column chromatography (Chromatorex NH; mobile phase: n-hexane/EtOAc=10/1 to 3/1; v/v) to obtain 3.94 g of the title compound (colorless powder).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08030499B2 |
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| Quelldatensatz | uspto-grants-2011_10 |
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| ORD ID | ord-ed2204e738f3451d964cad9d09492659 |
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| Quellennotiz | uspto-grants-2011_10 |
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