Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 2-Methylthiophene | HCID 11126 | — |
| Edukt | Methyl chloroglyoxylate | HCID 79846 | — |
| Edukt | Aluminum(III) Chloride | HCID 6451240 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 55268432 | HCID 55268432 | 99,8% |
Reaktionsschritte
To a suspension of aluminum trichloride (2.75 g, 20.6 mmol) and methyl 2-chloro-2-oxoacetate (1.90 mL, 20.7 mmol) in dry DCM (25 mL), cooled at 0° C. and under nitrogen atmosphere, is added 2-methylthiophene (1.00 mL, 10.33 mmol) dropwise. The reaction is stirred at RT for 15 hours. Then the mixture is cooled at 0° C., ice-water is slowly added and the organic phase is washed with aq. NaHCO3 and brine, dried over Na2SO4 and evaporated to obtain intermediate I266 as a brown oil (1.9 g, quantitative yield).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US08835682B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-7c5d0a31ffa3492c9161eb21654422d0 |
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| Quellennotiz | uspto-grants-2014_09 |
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