Reaktion #171958

ord-799a2ead17e84cfe838192fd9b6aae4c

Reaktionsbedingungen

Temperatur
130°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool to room temperature
  2. 2
    Sonstigethe resulting mass was triturated with acetone (25 ml) until a gray colored solid
  3. 3
    Sonstigeseparated
  4. 4
    SonstigeThe solid was collected by centrifugation
  5. 5
    Waschenwashed with acetone
  6. 6
    Sonstigedried under vacuum

Vorschrift

A mixture of Compound 3 (1.0 g, 3.4 mmol) and p-toluenesulfonic acid methyl ester (0.94 g, 5.1 mmol) was heated in a pressure tube at 130° C. for 1 hour. The mixture was allowed to cool to room temperature, and the resulting mass was triturated with acetone (25 ml) until a gray colored solid separated. The solid was collected by centrifugation, washed with acetone and dried under vacuum to yield 1.4 g (86%) of Compound 4 whose structure is given below:

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846952B2uspto-grants-2014_09