Reaktion #322854

ord-d87b8076768a42a2b6f35d56ff7a794b

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGthe mixture was stirred for 10 minutes at the same temperature
  2. 2
    FiltrationThe solid was filtered out from the reaction mixture
  3. 3
    Einengenthe filtrate was concentrated under reduced pressure
  4. 4
    workup.DISSOLUTIONThe obtained residue was dissolved in methylene chloride
  5. 5
    Trocknenthe solution was dried over anhydrous magnesium sulfate
  6. 6
    Einengenconcentrated under reduced pressure

Vorschrift

To a solution of 600 mg of (2RS)-2-cyclopentyl-2-methyl-5-hydroxy-6,7-dichloroindan-1-one (prepared by the method described in European Patent Publication No. 47011) in 6 ml of dry acetone was added 690 mg of potassium carbonate at a time and the mixture was stirred for twenty minutes. The reaction mixture was cooled to 0° C., 0.23 ml of trifluoromethanesulfonyl chloride was dropped thereto and the mixture was stirred for 10 minutes at the same temperature. The solid was filtered out from the reaction mixture and the filtrate was concentrated under reduced pressure. The obtained residue was dissolved in methylene chloride and the solution was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 860 mg of the title compound as crude product having the following physical data.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04640931uspto-grants-1987_02