Reaktion #1687629

ord-7657e5b7bf7749b5ade477c43dc5633b

Lösungsmittel

Reaktionsbedingungen

Temperatur
120°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling the mixture
  2. 2
    workup.ADDITIONwas poured over ice
  3. 3
    ExtraktionExtraction with 3×400 ml of dichloromethane
  4. 4
    Trocknendrying 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%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: USRE036374uspto-grants-1999_11