Reaktion #1747867

ord-3997275d56804cd7b800fc4a35bd29a2

Reaktionsgleichung

O=S1(=O)c2ccccc2N(c2ccc(OCc3ccccc3)cc2)c2ccccc21
10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide
O=C[O-].[NH4+]
ammonium formate
O=S1(=O)c2ccccc2N(c2ccc(O)cc2)c2ccccc21
10-(4-Hydroxyphenyl)phenothiazine 5,5-dioxide

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthe solution was filtered
  2. 2
    EinengenThe filtrate was concentrated
  3. 3
    workup.ADDITIONafter adding 10 ml of methanol
  4. 4
    FiltrationThe solid was filtered off with suction
  5. 5
    Waschenwashed with methanol
  6. 6
    Sonstigedried at 110° C. in a vacuum
  7. 7
    Sonstigedrying cabinet
  8. 8
    Sonstigewere obtained

Vorschrift

3.10 g (7.50 mmol) of 10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide, 2.30 g (35.7 mmol) of 98% ammonium formate and 7.5 g of 10% palladium on activated carbon were heated to boiling under reflux in 225 ml of acetone for 1 hour. After cooling to room temperature, the solution was filtered. The filtrate was concentrated and, after adding 10 ml of methanol, stirred overnight. The solid was filtered off with suction, washed with methanol and dried at 110° C. in a vacuum drying cabinet. 1.47 g (61% of theory) of analytically pure light gray microcrystals having an m.p. of 308-311° C. were obtained.

Quelle

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