Reaktion #1747868

ord-6c144124ca7c4974a84d4e5ac2edb506

Reaktionsgleichung

CCN(CC)CC
triethylamine
O=C(Cl)c1ccccc1
benzoyl chloride
O=S1(=O)c2ccccc2N(c2ccc(O)cc2)c2ccccc21
10-(4-hydroxyphenyl)phenothiazine 5,5-dioxide
O=C(Oc1ccc(N2c3ccccc3S(=O)(=O)c3ccccc32)cc1)c1ccccc1
4-(5,5-Dioxophenothiazin-10-yl)phenyl benzoate

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONthe solvent was distilled off
  2. 2
    workup.STIRRINGstirred at 75° C. for 30 min
  3. 3
    FiltrationThe solid was filtered off with suction while hot,
  4. 4
    Waschenwashed with hot water
  5. 5
    Sonstigedried at 120° C. in a forced-air drying cabinet
  6. 6
    Sonstigewere obtained

Vorschrift

0.68 g (6.68 mmol) of triethylamine and 0.34 g (2.44 mmol) of benzoyl chloride were added to a solution of 0.72 g (2.22 mmol) of 10-(4-hydroxyphenyl)phenothiazine 5,5-dioxide in 120 ml of acetonitrile. After stirring at room temperature for 45 min, the solvent was distilled off. The residue was taken up in 100 ml of hot water and stirred at 75° C. for 30 min. The solid was filtered off with suction while hot, washed with hot water and dried at 120° C. in a forced-air drying cabinet. 0.87 g (92% of theory) of colorless microcrystals having an m.p. of 233-235° C. were obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08029919B2uspto-grants-2011_10