Reaktion #1687629
ord-7657e5b7bf7749b5ade477c43dc5633b
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
120°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling the mixture
- 2workup.ADDITIONwas poured over ice
- 3ExtraktionExtraction with 3×400 ml of dichloromethane
- 4Trocknendrying of the combined organic phase over magnesium sulphate, and removal of the solvent in vacuo
Vorschrift
A mixture of 20 g (0.110 mol) of 73 and 100 ml of conc. sulphuric acid was heated to 120° C. for 4 h. After cooling the mixture was poured over ice followed by basification with ammonia. Extraction with 3×400 ml of dichloromethane, drying of the combined organic phase over magnesium sulphate, and removal of the solvent in vacuo gave crude 74 as a red oil, which was sufficiently pure. Yield: 17 g (0.100 mol, 97%).