Reaktionsgleichung
ClS(O)(=O)=O.[NH2:6][C:7]([CH2:14][CH3:15])([CH2:10][CH:11]=[CH:12][CH3:13])[CH2:8]O>C(#N)C>[CH2:10]([C:7]1([CH2:14][CH3:15])[CH2:8][NH:6]1)[CH:11]=[CH:12][CH3:13]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
Chlorosulphonic acid (18 mL) was added to a solution of the product from step (e) (32.3 g) in acetonitrile (100 ml) at least 9° C. When addition was complete, the mixture was warmed to room temperature. The resulting crystals were filtered off, washed with acetonitrile/pet. ether, dried, taken up in a mixture of 50% w/v aqu. KOH (100 mL) and water (55 mL) and distilled over KOH to give the desired product as a colourless oil (16.1 g). 1H NMR consistent with the proposed structure.
Aufarbeitung
- additionWhen addition
- filtrationThe resulting crystals were filtered off
- washwashed with acetonitrile/pet. ether
- customdried
- additiontaken up in a mixture of 50%
- distillationKOH (100 mL) and water (55 mL) and distilled over KOH
Quellen und Nachweise
- ORD-Eintrag
- ord-031db419b85e49eb8266022d09028e45
- Quelldatensatz
- uspto-grants-1998_03
- Patentnummer
- US05723458
Verknüpfte Notizen
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