Reaktion #4471

ord-76b14a9408c64659932b886070897fcf

Reaktionsgleichung

O=C1CCCc2[nH]c3ccc(F)cc3c21
product
O=C1CCCc2[nH]c3ccc(F)cc3c21
6-Fluoro-1,2,3,9-tetrahydro-4H-carbazol-4-one
O=C([O-])[O-].[K+].[K+]
potassium carbonate
COS(=O)(=O)OC
dimethylsulphate
Cn1c2c(c3cc(F)ccc31)C(=O)CCC2
title compound
Ausbeute 97.5%
Cn1c2c(c3cc(F)ccc31)C(=O)CCC2
6-Fluoro-1,2,3,9-tetrahydro-9-methyl-4H-carbazol-4-one
Ausbeute 97.5%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe mixture was concentrated to one half of its volume
  2. 2
    FiltrationThe mixture was filtered off
  3. 3
    Waschenwashed with water (50 ml)
  4. 4
    Sonstigeair-dried for 1 h
  5. 5
    Trocknendried in vacuo over phosphorus pentoxide

Vorschrift

The product of Stage (ii) (7.28 g), potassium carbonate (9.90 g), acetone (70 ml), and dimethylsulphate (5.1 ml) were vigorously stirred at room temperature overnight under nitrogen. The mixture was concentrated to one half of its volume and then stirred with water (350 ml) for 30 min. The mixture was filtered off, washed with water (50 ml), air-dried for 1 h, and dried in vacuo over phosphorus pentoxide to give the title compound as needles (7.59 g), m.p. 157.5°-158.5°.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04725615uspto-grants-1988_02